Process for Reducing Ethanol Loss While Developing Desirable Organoleptics During Wooden Barrel Aging of Alcoholic Beverage

ABSTRACT

An alcoholic beverage is aged in a wooden barrel after the barrel is covered by a film having an oxygen transmission rate of at least 50 cc/m 2 /day and an ethanol transmission rate of less than 30 g/m 2 /day. The beverage acquires one or more specific flavor components in an amount of 50%, 75%, or 100% relative to amounts of one or more of the same flavor components in a control alcoholic beverage aged in a wooden barrel without the film thereon. Covering the barrel with the film reduces the angels&#39; share evaporative loss, while allowing the beverage to develop desirable flavor components during aging. In another embodiment, the process reduces angels&#39; share evaporative loss while achieving organoleptics indistinguishable from a control.

This application claims priority from provisional U.S. Ser. No.61/847,803, filed 18 Jul. 2013, and U.S. Ser. No. 61/861,563, filed 2Aug. 2013, each of which is hereby incorporated, in its entirety, byreference thereto.

BACKGROUND

The present invention is directed to the wooden barrel aging ofalcoholic beverages such as distilled spirits, wine, and beer. Duringtypical wooden barrel aging of distilled spirits derived from grains andother farm sources, from 2 to 50 wt % or more of the distilled ethanoland water in the mixture diffuses between and through the wooden barrelcomponents (staves and heads) and thereafter evaporates into thesurrounding atmosphere. The diffusion and evaporation continuesthroughout the aging period, which can be from a few weeks or months upto 20 years or more. The extent of evaporation depends on the initialalcohol content of the distillate, the duration of aging in the woodenbarrels, relative humidity, ambient temperature, etc. The distilledspirits industry defines this loss as the “angels' share.”

The amount of water, ethanol, etc lost through evaporation when agingdistilled spirits in 53 gallon white oak barrels over periods of timeranging from 1 to 20+ years ranges from about 2% per year to about 10%per year, depending upon the ambient conditions during aging, e.g.,depending upon the climate. The distillate is considerably stronger uponemerging from the distillation process than it is after aging for 10years, as ethanol loss is greater than water loss. The loss of ethanolduring aging has adverse effects over and above the loss of the alcoholitself. The release of alcohol into the atmosphere around the barrelsproduces an explosion hazard, as the high ethanol content in the air canignite explosively if subjected to spark or flame. Evaporated ethanolreleased into the ambient environment also serves as sustenance forblack fungi and/or molds growing on warehouse walls, adjacent buildings,cars, etc.

For many decades, distillers have attempted to reduce the angels' shareduring aging of distilled spirits and wine in wooden casks. Barrels havebeen provided with coatings, including coating of the outer surface ofbarrel staves and/or barrel heads. Bonding agents have been used betweenthe staves. Barrels have been made from reconstructed staves havingintermediate plies of non-porous material. Barrels have been placedinside bags made from a multilayer film having an aluminum foil layerwith vinyl on each side, with the atmosphere evacuated and the bag heatsealed closed. Wooden barrels have been suspended in a secondarycontainer (e.g., metal barrel) over a reservoir of ethanol inside themetal barrel. Metal barrels containing distillate have been aged bysuspending wooden staves in the distillate, with oxygen supplied to thesystem. Finely pulverized wood has been added to distillate in acontainer to accelerate aging of the distillate. Aging of distillateshas also been accelerated by increasing the reaction of ethanol with theatmospheric oxygen. However, none of these solutions has proven tosignificantly reduce the Angels' Share while maintaining or improvingthe organoleptic properties of the alcoholic beverage. It would bedesirable to find a way to age alcoholic beverage in a manner allowingthe development of desirable organoleptic character while reducing lossdue to angels' share diffusion and evaporation.

SUMMARY

A process has been discovered to reduce the Angels' Share loss duringthe aging of alcoholic beverage products while maintaining or improvingthe organoleptic content of the alcoholic beverage.

A first aspect is directed to a process for aging an alcoholic beverage,comprising (a) filling a first wooden barrel with an unaged alcoholicbeverage, the barrel having an outer surface; (b) covering at least 60percent of the outer surface of the first wooden barrel with a filmhaving an oxygen transmission rate of at least 50 cc/m²/day and anethanol transmission rate of less than 30 g/m²/day; and (c) aging theunaged alcoholic beverage under ambient conditions while the alcoholicbeverage remains in the first wooden barrel surrounded by the film for atime period of at least 1 month, to produce an aged alcoholic beverage,wherein during aging, the alcoholic beverage acquires or produces atleast one flavor component selected from the group consisting ofvanillin, guaiacol, syringaldehyde, syringol, eugenol, isoeugenol,cis-β-methyl-γ-octalactone, o-cresol, 2-methoxy-4-methylphenol,4-methylsyringol, 4-ethylguaiacol, 4-vinylguaiacol, vanillyl methylketone, methoxyeugenol, sinapaldehyde, and furfural, so that the agedalcoholic beverage contains the at least one flavor component in anamount of at least 50% relative to an amount of the same flavorcomponent in a control alcoholic beverage aged in a control woodenbarrel without any film covering the control barrel during aging.

In an embodiment, at least 75% of the outer surface of the first woodenbarrel is covered with the film, and the aged alcoholic beveragecontains the at least one flavor component in an amount of at least 75%relative to the amount of the same flavor component in the controlalcoholic beverage.

In an embodiment, the aged alcoholic beverage contains each flavorcomponent in the group consisting of vanillin, guaiacol, syringaldehyde,syringol, eugenol, isoeugenol, cis-β-methyl-γ-octalactone, o-cresol,2-methoxy-4-methylphenol, 4-methylsyringol, 4-ethylguaiacol,4-vinylguaiacol, vanillyl methyl ketone, methoxyeugenol, sinapaldehyde,and furfural in an amount of at least 75% relative to the amount of eachcorresponding flavor component in the control alcoholic beverage.

In an embodiment, the film surrounds the outer surface of the firstwooden barrel, and the aged alcoholic beverage contains each flavorcomponent in the group consisting of each of syringol, eugenol,cis-β-methyl-γ-octalactone, o-cresol, 2-methoxy-4-methylphenol,4-methylsyringol, 4-ethylguaiacol, vanillyl methyl ketone, and furfuralin an amount of greater than 100% relative to the amount of eachcorresponding flavor component in the control alcoholic beverage. Forexample, if the aged alcohol beverage contains each of the flavorcomponents in an amount of 101% of the amount of the amount of each ofthe flavor components in the control, the process is in accordance withthis embodiment.

In an embodiment, the film surrounds the outer surface of the firstwooden barrel, and the film comprises cyclic olefin copolymer in anamount of from 15 to 80 weight percent, based on total film weight, andthe film has a thickness of from 1.5 to 6 mils, and the aged alcoholicbeverage contains eugenol in an amount of at least 110% relative to theamount of eugenol in the control alcoholic beverage. For example, if theaged alcohol beverage contains eugenol in an amount of 111% of theamount of the amount of eugenol in the control, the process is inaccordance with this embodiment.

In an embodiment, the film comprises cyclic olefin copolymer in anamount of from 15 to 80 weight percent, based on total film weight, andthe film has a thickness of from 1.5 to 6 mils and an ethanoltransmission rate of less than 1 g/m²/day and an oxygen transmissionrate of at least 170 cc/m²/day.

In an embodiment, the film is a multilayer film comprising polyolefin inan amount of from 50 to 82 percent, based on total film weight, andcyclic olefin copolymer in an amount of from 18 to 50 weight percentbased on total film weight, with the cyclic olefin copolymer beingpresent in a blend with polyolefin, the film having a thickness of from1.5 to 4 mils.

In an embodiment, the multilayer film comprises three layers includingtwo outer layers and one inner layer, the inner layer comprising a blendof from 20 to 80 wt % ethylene norbornene copolymer and from 80 to 20 wt% ethylene/alpha-olefin copolymer, and the alcoholic beverage product isselected from distillate and wine.

In an embodiment, barrel is surrounded by the film and the film has anethanol transmission rate of less than 1 g/m²/day and an oxygentransmission rate of at least 170 cc/m²/day and a moisture vaportransmission rate less than 1 g/m²/day, and the aged alcoholic beverage,either having an alcohol by volume of less than 30% or being dilutedwith water to have an alcohol by volume of 30%, exhibits an aroma andflavor, evaluated in accordance with ASTM E1879-00 Sensory Evaluation ofBeverages Containing Alcohol together with ASTM E1885-04 Standard Methodfor Sensory Analysis—Triangle Test, indistinguishable relative to thecontrol barrel containing the control alcoholic beverage.

In an embodiment, the inner layer comprises a blend of from 40 to 60 wt% ethylene norbornene copolymer and from 60 to 40 wt % polyolefin, andthe film has a thickness of from 2 to 3.5 mils and an ethanoltransmission rate of less than 0.5 g/m²/day and an oxygen transmissionrate of at least 170 to 250 cc/m²/day, and the first aged alcoholicbeverage, either having an alcohol by volume of less than 30% or beingdiluted with water to have an alcohol by volume of 30%, further exhibitsa color, evaluated in accordance with ASTM E1879-00 Sensory Evaluationof Beverages Containing Alcohol, together with ASTM E1885-04 StandardMethod for Sensory Analysis—Triangle Test, indistinguishable relative tothe control barrel containing the control alcoholic beverage.

A second aspect is directed to a process for aging an alcoholicbeverage, comprising (a) filling a first wooden barrel with an unagedalcoholic beverage, the barrel having an outer surface; (b) covering atleast 60 percent of the outer surface of the first wooden barrel with afilm having an oxygen transmission rate of at least 50 cc/m²/day and anethanol transmission rate of less than 30 g/m²/day; and (c) aging theunaged alcoholic beverage in the first wooden barrel covered with thefilm, the aging being carried out under ambient conditions for a timeperiod of at least 1 month while the alcoholic beverage remains in thefirst wooden barrel covered by the film, to produce an aged alcoholicbeverage, wherein during aging, an angel share fraction of the alcoholicbeverage escapes through the wooden barrel and through the film coveringthe outer surface of the wooden barrel, with the angel share fractionbeing at least 30% less relative to a corresponding angel share fractionescaping through a wooden control barrel containing a control alcoholicbeverage aged in the control barrel, the control barrel having an outersurface in direct contact with an ambient atmosphere without any filmcovering any portion of the control barrel. The aged alcoholic beverage,either having an alcohol by volume of less than 30% or upon beingdiluted with water to have an alcohol by volume of 30%, exhibits anaroma and flavor, upon evaluation in accordance with ASTM E1879-00Sensory Evaluation of Beverages Containing Alcohol together with ASTME1885-04 Standard Method for Sensory Analysis—Triangle Test, isindistinguishable relative to the control barrel containing the controlalcoholic beverage aged therein, the aged control alcoholic beveragealso having an alcohol by volume of less than 30% or being diluted withwater to have an alcohol by volume of 30%.

In an embodiment, the first barrel is surrounded by the film and theangels' share is reduced by at least 70% relative to the control barrelcontaining the control alcoholic beverage, and the film comprisespolyolefin.

In an embodiment, the first barrel is surrounded by the film and theangels' share is reduced by at least 85% relative to the control barrelcontaining the control alcoholic beverage, and the film comprises from30 to 85 wt % polyolefin and from 70 to 15 wt % ethylene/norbornenecopolymer based on total film weight, and the film has an oxygentransmission rate of from 170 to 350 cc/m²/day and an ethanoltransmission rate of from 0.10 to 1.0 g/m²/day.

In an embodiment, the angels' share is reduced by at least 90% relativeto the control barrel containing the control alcoholic beverage, and thefilm comprises from 40 to 60 wt % polyolefin and from 60 to 40 wt %ethylene/norbornene copolymer based on total film weight, and the filmhas an oxygen transmission rate of from 170 to 250 cc/m²/day and anethanol transmission rate of from 0.17 to 0.27 g/m²/day, and the agedalcoholic beverage, either having an alcohol by volume of less than 30%or being diluted with water to have an alcohol by volume of 30%, furtherexhibits a color, evaluated in accordance with ASTM E1879-00 SensoryEvaluation of Beverages Containing Alcohol, together with ASTM E1885-04Standard Method for Sensory Analysis—Triangle Test, indistinguishablerelative to the control barrel containing the control alcoholicbeverage.

A third aspect is directed to a process for aging an alcoholic beverage,comprising (a) filling a wooden barrel with an unaged alcoholicbeverage, the wooden barrel having an oxygen transmission rate of from 1to 10 cc/m²/day, (b) covering an outer surface of the barrel with a filmhaving an oxygen transmission rate of at least 50 cc/m²/day and anethanol transmission rate of less than 30 g/m²/day, the film having athickness of from 1 to 10 mils, and (c) aging the unaged alcoholicbeverage while it remains in the wooden barrel, covered by the film, forat least 1 month, to produce an aged alcoholic beverage.

In an embodiment, the film has an oxygen transmission rate of at least100 cc/m²/day and an ethanol transmission rate of from 0.1 to 20g/m²/day, and the film comprises polyolefin.

In an embodiment, the film has a thickness of from 1.5 to 5 mils.

In an embodiment, the film has an oxygen transmission rate of at least120 cc/m²/day and an ethanol transmission rate of 0.1 to 1 g/m²/day, andthe film further comprises a cyclic olefin copolymer, and the aging ofthe alcoholic beverage is carried out for at least 2 months.

In an embodiment, the film further comprises a blend of the polyolefinand the cyclic olefin copolymer, and the cyclic olefin copolymercomprises ethylene/norbornene copolymer, and the ethylene norbornenecopolymer is present in the film in an amount of from 15 to 70 weightpercent based on total film weight and the polyolefin is present in thefilm in an amount of from 30 to 85 wt % based on total film weight, andthe aging of the alcoholic beverage is carried out for at least 3months, and the film has a thickness of from 2 to 4 mils, an oxygentransmission rate of from 150 to 500 cc/m²/day, an ethanol transmissionrate of less than 1 g/m²/day, and a moisture vapor transmission rateless than 1 g/m²/day.

A fourth aspect is directed to a product suitable for aging, comprising(a) an unaged alcoholic beverage inside a wooden barrel, the woodenbarrel surrounding the alcoholic beverage and the wooden barrel havingan oxygen transmission rate of from 1 to 10 cc/m²/day, and (b) a filmcovering at least 60 percent of an outer surface of the barrel, the filmhaving an oxygen transmission rate of at least 50 cc/m²/day and anethanol transmission rate of less than 30 g/m²/day, a moisture vaportransmission rate less than 1 g/m²/day, and a peak load impact strengthof at least 100 Newtons, a thickness of from 1 to 10 mils.

In an embodiment, the film surrounds the barrel and the film comprisescyclic olefin copolymer in an amount of from 15 to 80 wt %, based ontotal film weight, the film has an ethanol transmission rate of lessthan 1 g/m²/day, the film has an oxygen transmission rate of from 175 to350 cc/m²/day, the film has a peak load impact strength of from 150 to200 Newtons, and the film has a total thickness of from 2 to 4 mils.

In a fifth aspect directed to a film suitable for use in aging an unagedalcoholic beverage in a wooden barrel with the film covering an outersurface of the wooden barrel, the film comprises a blend of polyolefinand cyclic olefin copolymer, the cyclic olefin copolymer comprisingethylene/norbornene copolymer, with the ethylene norbornene copolymerbeing present in the film in an amount of from 15 to 70 weight percentbased on total film weight, and the polyolefin being present in the filmin an amount of from 30 to 85 wt % based on total film weight, with thefilm having a peak load impact strength of at least 100 Newtons, athickness of from 2 to 4 mils, an oxygen transmission rate of from 150to 500 cc/m²/day, an ethanol transmission rate of less than 1 g/m²/day,and a moisture vapor transmission rate of less than 1 g/m²/day.

In a sixth aspect directed to a film for use in aging an imagedalcoholic beverage in a wooden barrel with the film covering an outersurface of the wooden barrel, the film comprises polyolefin in an amountof from 80 to 100 weight percent based on total film weight, the filmhaving a thickness of from 2 to 4 mils, an oxygen transmission rate offrom 150 to 500 cc/m²/day, an ethanol transmission rate of less than 30g/m²/day, a moisture vapor transmission rate less than 1 g/m²/day, andthe film having a peak load impact strength of at least 100 Newtons.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG. 1 is a schematic plan view of an end-seal bag.

FIG. 2 is a transverse cross-sectional view of the end-seal bag of FIG.1, taken through section 2-2 of FIG. 1.

FIG. 3 is a schematic plan view of a side-seal bag.

FIG. 4 is a transverse cross-sectional view of the side-seal bag of FIG.3, taken through section 4-4 of FIG. 3.

FIG. 5 is a schematic plan view of an L-seal bag.

FIG. 6 is a transverse cross-sectional view of the L-seal bag of FIG. 5,taken through section 6-6 of FIG. 5.

FIG. 7 is a longitudinal cross-sectional view of the L-seal bag of FIG.5, taken through section 7-7 of FIG. 5.

FIG. 8 is a schematic plan view of a backseamed bag having a fin-typebackseam.

FIG. 9 is a transverse cross-sectional view of the backseamed bag ofFIG. 8.

FIG. 10 is a schematic plan view of a backseamed bag having a lap-typebackseam.

FIG. 11 is a transverse cross-sectional view of the backseamed bag ofFIG. 10.

FIG. 12 is a schematic plan view of a pouch-type bag.

FIG. 13 is a transverse cross-sectional view of the pouch-type bag ofFIG. 12, taken through section 13-13 of FIG. 12.

FIG. 14 is a longitudinal cross-sectional view of the pouch-type bag ofFIG. 12, taken through section 14-14 of FIG. 12.

FIG. 15 is a schematic of a process used to make a heat-shrinkable filmsuch as could be used to make a heat-shrinkable bag.

FIG. 16 is a schematic of a process used to make a non-heat-shrinkablefilm that can be used to make a non-heat-shrinkable bag.

FIG. 17 is a schematic of a barrel enveloped within a bag that has beensealed closed.

FIG. 18 is a schematic of a process for measuring the ethanoltransmission rate of a film.

FIG. 19 is a graph of weight loss as a function of time for pouches madefrom Film No. 22, under two different relative humidity conditions.

FIG. 20 is a graph of weight loss as a function of time for pouches madefrom Film No. 21, under two different relative humidity conditions.

FIG. 21 is a graph of weight loss as a function of time for pouches madefrom Film No. 20, under two different relative humidity conditions.

FIG. 22 is a graph of weight loss as a function of time for pouches madefrom Film No. 17, under two different relative humidity conditions.

FIG. 23 is a graph of weight loss as a function of time for pouches madefrom Film No. 18, under two different relative humidity conditions.

FIG. 24 is a graph of weight loss as a function of time for pouches madefrom Film No. 19, under two different relative humidity conditions.

FIG. 25 is a graph of weight loss as a function of time for a 95%ethanol solution in pouches made from Film Nos. 17-22, under twodifferent relative humidity conditions.

FIG. 26 is a graph of weight loss as a function of time for a 100% waterin pouches made from Film Nos. 17-22, under two different relativehumidity conditions.

FIG. 27 is a graph of weight loss as a function of time for a 57%/43%ethanol/water solution in pouches made from Film Nos. 17-22, under twodifferent relative humidity conditions.

FIG. 28 is a graph of weight loss as a function of time for a 95%ethanol solution in pouches made from Film No. 22 overpouched withvarious sizes of overpouches made from Film 20 and Film 22.

FIGS. 29 through 45 provide GC/MS data of various flavor componentspresent in aged Virgin Wheat Whisky aged under a variety of conditions.

DETAILED DESCRIPTION

As used herein, the term “barrel” refers to wooden barrels as used forthe aging of distillate alcoholic beverages, wine, and beer. As usedherein, the phrase “wooden barrel” refers to a barrel having at leastone wooden stave or at least one wooden cant in the head. As usedherein, the term “cask” is used interchangeably with the word “barrel.”The barrel can be of any desired size, from a quart (or liter) or evenless, to 250 gallons (1000 liters) or more. In an embodiment the woodcomprises oak, and in a further embodiment, white oak. At least aportion of the interior surface of the barrel is charred.

As used herein, the phrase “filling a barrel” includes partial fillingof the barrel as well as filling the barrel to the maximum. Usually,filling of the barrel is to the maximum.

Oak barrels generally have an oxygen transmission rate (OTR) of fromapproximately 2.5 to 4 cc/m²/day, which varies with ambient conditionssuch as temperature, relative humidity, thickness of wood, amount ofliquid inside barrel, etc. and relative humidity. The aging of alcoholicbeverages benefits from an OTR of 2.5 to 4 cc/m²/day over the surface ofthe barrel, as the beverage inside the barrel needs a net transmissionof oxygen into the barrel (i.e., inward, through the staves and ends) inorder to support the oxidative reactions needed for the generation ofthe desired flavor profiles as the alcoholic beverage ages.

As used herein, the phrase “covering . . . the barrel with a film”refers to placing a film over at least a portion of the outer surface ofthe barrel, such as covering at least 60% of the outer surface of thebarrel, or even covering 100% of the outer surface of the barrel. Asused herein, the phrase “surrounding . . . the barrel with a film”refers to 100% coverage of the outer surface of the barrel. The film canprovide 100% coverage of the barrel regardless of whether the film istight or loose around the barrel. Films can be used to cover only theouter surfaces of the barrel staves with the barrel ends left uncovered,or films can be used to cover the barrel ends only, leaving the outersurface of the barrel staves left uncovered.

The wooden barrel can be covered by a first film and a second film, withthe first film being between the wooden barrel and the second film. Thesecond film can have a thickness of from 1 to 20 mils. The second filmcan exhibit a peak load impact strength of from 30 to 200 poundsmeasured in accordance with ASTM D 3763, which is hereby incorporated,in its entirety, by reference thereto. The second film can have athickness of from 3 to 20 mils, the second film exhibiting a peak loadimpact strength of from 50 to 200 pounds measured by the procedure ofASTM D 3763. The second film can have a thickness of from 1 to 2.9 mils,and the second film can exhibit a peak load impact strength of from 30to 65 pounds measured by the procedure of ASTM D 3763. The packagedalcoholic beverage product can further comprise a protective plasticmesh over the film or films covering the wooden staves of the barrel,with the plastic mesh also covering the hoops of the barrel.

In an embodiment, the entire exterior surface of the staves can becovered by the film, with the barrel ends uncovered. In an alternativeembodiment, one or both of the barrel ends are covered by the film, withthe exterior surface of the staves left uncovered.

In an embodiment, both the staves and the hoops are covered by the film.In an alternative embodiment, the film is between the staves and thehoops.

If a barrel is covered with a film within a specified thickness range,the film can be a single discrete film within the thickness range, orthe film can be the sum of the thickness of a thin film wrapped multipletimes over top of itself and over the barrel to generate a total filmthickness within the specified thickness range.

As used herein, the term “film” is used in a generic sense to includeplastic web, regardless of whether it is film or sheet. Preferably,films of and used in the present invention have a thickness of 0.25 mmor less. The film can have any total thickness desired, so long as thefilm provides the desired properties for the particular packagingoperation in which the film is used.

Moreover, the film is inclusive of both a free standing film and acoating film. The phrase “free-standing film,” as used herein, refers toa film made from one or more layers which have been extruded through adie. As used herein, the phrase “coating film” refers to a film appliedto a surface by spray coating, dipping, or a coating applied with anapplicator such as a brush, cloth, spatula, etc. In accordance with anyone or more of the above aspects, as well as any one or more of theembodiments of those aspects, the film can be a free standing film or acoating film.

As used herein, the phrase “oxygen transmission rate” and the phrase “O₂transmission rate” and the acronym “OTR” all refer to the rate at whichatmospheric O₂ (i.e., O₂ gas) is transmitted through a film using themeasurement process of ASTM D3985-05 (2010)e1, which is herebyincorporated, in its entirety, by reference thereto. This is sometimesalso referred to as “oxygen gas transmission rate” with the acronym“O₂GTR.” Oxygen transmission rate and oxygen gas transmission rate canboth expressed in the units of cubic centimeters per square meter offilm per day. Each of the expressions “cc/m² day” and “cc/m²/day” areconsidered to represent “cubic centimeters per square meter of film perday.” The measurement is carried out at standardized conditions of 1atmosphere pressure, 23° C., and 0% relative humidity.

Unless otherwise excluded in an above aspect or embodiment thereof, in afurther embodiment of any of the above aspects and embodiments, the filmcan have an oxygen transmission rate of at least 60 cc/m²/day, or atleast 70 cc/m²/day, or at least 80 cc/m²/day, or at least 90 cc/m²/day,or at least 100 cc/m²/day, or at least 110 cc/m²/day, or at least 120cc/m²/day, or at least 130 cc/m²/day, or at least 140 cc/m²/day, or atleast 150 cc/m²/day, or at least 160 cc/m²/day, or at least 170cc/m²/day, or at least 180 cc/m²/day, or at least 190 cc/m²/day, or atleast 200 cc/m²/day. The film can have an oxygen transmission rate offrom 50 to 2000 cc/m²/day, or from 60 to 1800 cc/m²/day, or from 70 to1700 cc/m²/day, or from 80 to 1500 cc/m²/day, or from 80 to 1200cc/m²/day, or from 80 to 1000 cc/m²/day, or from 80 to 800 cc/m²/day, orfrom 80 to 700 cc/m²/day, or from 80 to 600 cc/m²/day, or from 80 to 500cc/m²/day, or from 90 to 450 cc/m²/day, or from 100 to 400 cc/m²/day, orfrom 110 to 375 cc/m²/day, or from 120 to 350 cc/m²/day, or from 130 to350 cc/m²/day, or from 140 to 350 cc/m²/day, or from 150 to 350cc/m²/day, or from 160 to 340 cc/m²/day, or from 170 to 330 cc/m²/day,or from 180 to 320 cc/m²/day, or from 190 to 310 cc/m²/day, or from 200to 300 cc/m²/day.

As used herein, the phrase “moisture vapor transmission rate” and theacronym “MVTR” refer to the rate at which atmospheric moisture istransmitted through a film using the measurement process of ASTM F1249-06 (2011)e1, which is hereby incorporated, in its entirety, byreference thereto. The phrase “water vapor transmission rate” and theacronym “WVTR” are also used interchangeably with MVTR. The moisturevapor transmission rate can be expressed as grams per 100 square inchesof film per day. Each of the expressions “g/100 in² day” and “g/100in²/day” are considered to represent “grams per 100 square inches offilm per day.” The measurement is carried out at standardized conditionsof 1 atmosphere pressure, 100° F. (37.8° C.), and 100% relativehumidity.

Unless otherwise excluded in an above aspect or embodiment thereof, in afurther embodiment of any of the above aspects and embodiments, the filmcan have an moisture vapor transmission rate of less than 15 g/m²/day,or less than 12 g/m²/day, or less than 10 g/m²/day, or less than 9g/m²/day, or less than 8 g/m²/day, or less than 7 g/m²/day, or less than6 g/m²/day, or less than 5 g/m²/day, or less than 4 g/m²/day, or lessthan 3 g/m²/day, or less than 2.5 g/m²/day, or less than 2 g/m²/day, orless than 1.5 g/m²/day, or less than 1.4 g/m²/day, or less than 1.3g/m²/day, or less than 1.2 g/m²/day, or less than 1.1 g/m²/day, or lessthan 1 g/m²/day, or less than 0.9 g/m²/day, or less than 0.8 g/m²/day,or less than 0.7 g/m²/day, or less than 0.6 g/m²/day, or from 0.1 to 30g/m²/day, or from 0.15 to 15 g/m²/day, or from 0.2 to 12 g/m²/day, orfrom 0.2 to 11 g/m²/day, or from 0.3 to 10 g/m²/day, or from 0.3 to 8g/m²/day, or from 0.3 to 6 g/m²/day, or from 0.3 to 5 g/m²/day, or from0.3 to 4 g/m²/day, or from 0.3 to 3 g/m²/day, or from 0.3 to 2 g/m²/day,or from 0.3 to 1.5 g/m²/day, or from 0.35 to 1 g/m²/day, or from 0.35 to0.9 g/m²/day, or from 0.35 to 0.8 g/m²/day, or from 0.4 to 0.7 g/m²/day,or from 0.45 to 0.65 g/m²/day.

As used herein, the phrase “ethanol transmission rate” and the acronym“ETR” each refer to the rate at which ethanol is transmitted through afilm, and is measured using a cell in which the film is installed withan excess of ethanol in the bottom of the cell (below the film), with astream of ethanol-free nitrogen constantly purging the top of the cell(above the film) at a low rate, e.g., 10 cc dry nitrogen per minute. Thecell has mating surfaces in a clamshell arrangement, with the filminstalled between the mating surfaces so that the volume inside the cellis sealed except for the inlet and outlet ports for insertion of thestream of nitrogen gas. Those of skill in the art know that this type ofarrangement is present in Mocon® Ox-Tran® instruments used for measuringoxygen transmission rate through a film.

Conceptually, the test cell is illustrated in FIG. 19, with dry nitrogenbeing swept through the portion of the chamber above the film. Thepartial pressure difference between the high-ethanol concentrationatmosphere below the film and the lower ethanol concentration atmosphereabove the film causes ethanol molecules to diffuse through the film intothe low concentration atmosphere above the film. The use of the purginggas in that portion of the chamber above the film maintains the lowethanol concentration in the atmosphere above the film in order tomaintain a constant rate of diffusion of the ethanol through the film.

The ethanol barrier character of the film determines the rate of ethanolpermeation, which can be continuously measured from the outflow of thenitrogen gas sweeping through that portion of the chamber containing theatmosphere above the film. A steady state is eventually reached in theatmosphere above the film. This steady state can require days or weeksto achieve. A steady state is reached when the sensor used detects aconstant (i.e., unchanging) amount of ethanol in the atmosphere sweptout of the upper portion of the chamber. The response is never trulyconstant or unchanging; it merely reaches a state in which the change insignal versus time is below some defined threshold. Initially the signalwill change greatly with time but will eventually reach a point whereΔsignal/Δtime is significantly lower. At steady state, by definition theamount of ethanol purged out of the upper portion of the chamber in agiven time corresponds precisely with the amount of ethanol passingthrough the film during the same period of time. The amount of ethanolpassing through the film in any given period of time divided by the areaof the film being tested is the calculation of the transmission rate ofethanol through a specified area of film in a specified period of time.This transmission rate can be expressed in terms such as grams ethanolper square meter per day (i.e., g/m²/day, also expressed as g/m² day).The transmission rate can also be normalized for the film thickness,e.g., g/100μ/m²/day, as reported in examples below.

FIG. 18 illustrates the process and equipment for the evaluation of theETR of a film sample for use in a film covering part or all of a woodenbarrel containing an alcoholic beverage such as a distillate product,wine, or beer. In FIG. 18, film sample 172 is held in permeation cell170 between lower cell member 174 and upper cell member 176. Pool 178 of95% ethanol solution is contained with a recess formed inside lowermember 174. Ethanol vapor evaporating from pool 178 passes intoatmosphere 180 above the upper surface of pool 178 but below film sample172.

Ethanol vapor in atmosphere 180 below film sample 172 permeates filmsample 172, moving into chamber upper volume 184 which is bounded byfilm sample 172 and inside surface 186 of upper cell member 176. Therate of ethanol permeation through film sample 172 is measured bycontinuously flushing upper chamber volume 184 with nitrogen gas, withthe ethanol content of the gas emerging from upper volume 184 beingintermittently sampled and analyzed. The analysis can be carried out bypassing the sample into an analytical device such as a gas chromatograph(schematically illustrated as 186), equipped with, for example, a flameionization detector (FID, not illustrated). The ethanol is separatedfrom any other components emerging, and then passes through the FID,which generates a peak corresponding to the amount of ethanol in thesample. In this manner, the amount of ethanol emerging from the uppervolume can be determined, and in so doing the ethanol transmission rateof the film can be measured.

In place of a flame ionization detector or other detector in the gaschromatograph, the ethanol separated in the gas chromatograph can bepassed through a Mass Spectrometer Detector (MSD) 188. As such, theethanol flushed from upper chamber volume 184 is separated from othercomponents using capillary column gas chromatograph 186 and isthereafter both identified and quantified by the character and intensityof the mass spectral fragmentation pattern generated by the massspectrometer, resulting in the identification and quantification of theethanol contained in the stream emerging from upper chamber volume 184.

This type of ethanol transmission rate measurement has been used for theethanol transmission rates reported herein. These ethanol transmissionrates were measured by Mocon Inc., at 7500 Mendelssohn Avenue N.,Minneapolis, Minn. 55428. The ethanol transmission rate is set forth inthe normalized-for-film-thickness units of “g/100μ/m² day.” The analysisis conducted while the film was in an ambient environment at 38-40° C.The analysis was carried out until steady state was reached, or for 4weeks, whichever was shorter. Macon reports that they use a capillarychromatography column in an Agilent 6890 gas chromatograph equipped withan FID.

Unless otherwise excluded in an above aspect or embodiment thereof, in afurther embodiment of any of the above aspects and embodiments, the filmcan have an ethanol transmission rate of less than 25 g/m²/day, or lessthan 20 g/m²/day, or less than 15 g/m²/day, or less than 10 g/m²/day, orless than 8 g/m²/day, or less than 6 g/m²/day, or less than 5 g/m²/day,or less than 4 g/m²/day, or less than 3 g/m²/day, or less than 2.5g/m²/day, or less than 2 g/m²/day, or less than 1.5 g/m²/day, or lessthan 1.4 g/m²/day, or less than 1.3 g/m²/day, or less than 1.2 g/m²/day,or less than 1.1 g/m²/day, or less than 1.0 g/m²/day, or less than 0.9g/m²/day, or less than 0.8 g/m²/day, or less than 0.7 g/m²/day, or lessthan 0.6 g/m²/day, or less than 0.5 g/m²/day, or less than 0.4 g/m²/day,or less than 0.3 g/m²/day, or less than 0.25 g/m²/day. The film can havean ethanol transmission rate of from 0.05 to 40 g/m²/day, or from 0.1 to35 g/m²/day, or from 0.2 to 1 g/m²/day, or from 0.11 to 30 g/m²/day, orfrom 0.12 to 25 g/m²/day, or from 0.13 to 20 g/m²/day, or from 0.14 to15 g/m²/day, or from 0.15 to 10 g/m²/day, or from 0.15 to 8 g/m²/day, orfrom 0.15 to 6 g/m²/day, or from 0.15 to 4 g/m²/day, or from 0.15 to 2g/m²/day, or from 0.16 to 1.5 g/m²/day, or from 0.17 to 1.4 g/m²/day, orfrom 0.18 to 1.3 g/m²/day, or from 0.19 to 1.2 g/m²/day, or from 0.2 to1 g/m²/day.

Unless otherwise excluded in an above aspect or embodiment thereof, in afurther embodiment of any of the above aspects and embodiments, the filmcan have a peak load impact strength (measured in accordance with ASTM D3763, which is hereby incorporated, in its entirety, by referencethereto) of at least 100 Newtons, or at least 110 Newtons, or at least120 Newtons, or at least 130 Newtons, or at least 140 Newtons, or atleast 150 Newtons, or from 100 to 1000 Newtons, or from 110 to 600Newtons, or from 120 to 500 Newtons, or from 130 to 400 Newtons, or from140 to 300 Newtons, or from 145 to 290 Newtons.

Unless otherwise excluded in an above aspect or embodiment thereof, in afurther embodiment of any of the above aspects and embodiments, the filmcan have an elongation to break (measured in accordance with ASTM D882,which is hereby incorporated, in its entirety, by reference thereto) ofat least 0.5 Joule, or at least 0.7 Joule, or at least 1 Joule, or atleast 1.3 Joules, or at least 1.5 Joules, or at least 1.6 Joules, or atleast 1.7 Joules, or at least 1.8 Joules, or at least 1.9 Joules, or atleast 2 Joules, or from 1.7 to 4 Joules, from 1.7 to 4.1 Joules, or from1.7 to 4 Joules, or from 1.7 to 3.5 Joules, or from 1.7 to 3 Joules, orfrom or from 1.7 to 2.5 Joules, or from 1.7 to 2.3 Joules, or from 1.7to 2.2 Joules.

As used herein, the phrase “free shrink” refers to the percentdimensional change in a 10 cm. by 10 cm. specimen of film, whensubjected to selected heat (i.e., at a certain temperature), with thequantitative determination being carried out according to ASTM D 2732,as set forth in the 1990 Annual Book of ASTM Standards, Vol. 08.02, pp.368-371, which is hereby incorporated, in its entirety, by referencethereto. The test is carried out under designated conditions, i.e., oneatmosphere of pressure, 23° C., and 0% relative humidity.

As used herein, the phrase “machine direction”, herein abbreviated “MD”,refers to a direction “along the length” of the film, i.e., in thedirection of the film as the film is formed during extrusion and/orcoating. As used herein, the phrase “transverse direction”, hereinabbreviated “TD”, refers to a direction across the film, perpendicularto the machine or longitudinal direction.

In an embodiment, the film has a total free shrink (longitudinal plustransverse) at 185° F. of at least 10 percent, measured in accordancewith ASTM D 2732. The film can have a total free shrink at 185° F. of atleast 30 percent, measured in accordance with ASTM D 2732. The film canhave a total free shrink at 185° F. of at least 50 percent, measured inaccordance with ASTM D 2732. In an embodiment, the film has a total freeshrink at 185° F. of less than 10 percent, measured in accordance withASTM D 2732.

Unless otherwise excluded in an above aspect or embodiment thereof, in afurther embodiment of any of the above aspects and embodiments, the filmcan have thickness (i.e., total film thickness) of from 1 mil to 20mils, or from 1.2 mils to 15 mils, or from 1.3 mils to 12 mils, or from1.4 mils to 10 mils, or from 1.5 mils to 8 mils, or from 1.6 mils to 7mils, or from 1.7 mils to 6.5 mils, or from 1.8 mils to 6 mils, or from1.9 mils to 5.5 mils, or from 2 mils to 5 mils, or from 2.5 to 4 mils,or from 2.5 to 3.5 mils, or from 2.7 to 3.3 mils.

The film can be a monolayer film or a multilayer film. In an embodiment,the film comprises a first layer that is an inner film layer serves asan ethanol barrier layer, a second layer that is a first outer filmlayer and which serves as a heat seal layer, and a third layer which isa second outer film layer and which serves as an abuse layer.

As used herein, the term “heat-seal,” and the phrase “heat-sealing,”refer to any seal of a first discrete region of a film surface to asecond discrete region of a film surface, wherein the heat seal isformed by heating the discrete regions to at least their respective sealinitiation temperatures. Suitable polymers for use in heat seal layershomogeneous ethylene/alpha-olefin copolymer, ethylene/vinyl acetatecopolymer, and ionomer resin.

The layer which is a barrier to ethanol can comprise a cyclic olefinpolymer (COP) or including a cyclic olefin copolymer (COC). There arevarious types of cyclic olefin copolymers based on different types ofcyclic monomers and polymerization methods. Cyclic olefin copolymers areproduced by chain copolymerization of cyclic monomers such as8,9,10-trinorborn-2-ene (norbornene) or1,2,3,4,4a,5,8,8a-octahydro-1,4:5,8-dimethanonaphthalene(tetracyclododecene) with ethene, or by ring-opening metathesispolymerization of various cyclic monomers followed by hydrogenation.These latter materials using a single type of monomer are more properlynamed cyclic olefin polymers.

The cyclic olefin copolymer can comprise ethylene/norbornene copolymer.Cyclic olefin copolymer is a barrier to both ethanol and water vapor.Alternatively, polyolefin provides a relatively high barrier to moisturevapor, but is a lesser barrier to ethanol than is cyclic olefincopolymer.

As used herein, the term “polyolefin” refers to all polymerized olefinsexcept cyclic olefin copolymers such as ethylene/norbornene. Included aslinear, branched, aliphatic, aromatic, substituted, or unsubstituted.More specifically, included in the term polyolefin are homopolymers ofolefin, copolymers of olefin, copolymers of an olefin and annon-olefinic comonomer copolymerizable with the olefin, such as vinylmonomers, modified polymers thereof, and the like. Specific examplesinclude polyethylene homopolymer, polypropylene homopolymer, polybutene,ethylene/alpha-olefin copolymer, propylene/alpha-olefin copolymer,butene/alpha-olefin copolymer, ethylene/unsaturated ester copolymer,ethylene/unsaturated acid copolymer, (especially ethyl acrylatecopolymer, ethylene/butyl acrylate copolymer, ethylene/methyl acrylatecopolymer, ethylene/acrylic acid copolymer, ethylene/methacrylic acidcopolymer), modified polyolefin resin, ionomer resin, polymethylpentene,etc. Modified polyolefin resin is inclusive of modified polymer preparedby copolymerizing the homopolymer of the olefin or copolymer thereofwith an unsaturated carboxylic acid, e.g., maleic acid, fumaric acid orthe like, or a derivative thereof such as the anhydride, ester or metalsalt or the like. It could also be obtained by incorporating into theolefin homopolymer or copolymer, an unsaturated carboxylic acid, e.g.,maleic acid, fumaric acid or the like, or a derivative thereof such asthe anhydride, ester or metal salt or the like.

In a film having at least one layer containing a cyclic olefincopolymer, one or more additional layers of the film can be made from apolymer allowing relatively high transmission of atmospheric oxygen(i.e., O₂), such as polyolefins including ethylene homopolymer,ethylene/α-olefin copolymer, propylene homopolymer, etc. In this mannerthe transmission rate of alcohol and water can be reduced in combinationwith providing a high oxygen transmission rate while at the same timeproviding a film of high peak load impact strength.

The film can comprise up to 100 weight percent polyolefin. The film cancomprise up to 90 weight percent cyclic olefin copolymer, e.g.,ethylene/norbornene copolymer. The film can comprise a blend ofpolyolefin and cyclic olefin copolymer.

In an embodiment of each of the above aspects (including embodimentsthereof), the film does not comprise, and is absent, polyphenylenesulfide.

In an embodiment of each of the above aspects (including embodimentsthereof), the film does not comprise, and is absent, a metal foil layeror a vapor deposited metal layer.

In an embodiment of each of the above aspects (including embodimentsthereof), the film does not comprise, and is absent, aluminum foil.

In an embodiment of each of the above aspects (including embodimentsthereof), the film does not comprise, and is absent, polyvinylchloride.

In an embodiment, the film is a stretch film. A stretch film and/orelastic film can have a thickness of from about 0.5 mil to 5.0 mil, anelongation of 500%, and an elastic recovery of at least 10%.

In an embodiment, the film comprises an ultraviolet light barrier,including, for example, hindered amine light stabilizers (HALS),benzotriazoles, and hydroxyl-benophenones.

In an embodiment, the film comprises an antioxidant, including, forexample, sterically hindered phenolic antioxidant, for example IRGANOX®1010 or IRGANOX® 1076 and, phosphorous phosphite compounds like IRGAFOS®168(tris(2,4-di-tert-butylphenyl)phosphite.)

The alcoholic beverage can comprise at least one member selected from adistilled alcoholic beverage product and a fermented alcoholic beverageproduct. The alcoholic beverage product can comprise wine. The alcoholicbeverage product can comprise beer. In an embodiment, the alcoholicbeverage product comprises at least one member selected from the groupconsisting of whisky, tequila, rum, cognac, vodka, brandy, sherry, port,wine, and beer. Distillate alcoholic beverage products include whisky,cognac, brandy, sherry, and port. Alcoholic beverages include both waterand ethanol.

As used herein, the phrase “unaged alcoholic beverage” includesalcoholic beverages which are entirely unaged, as well as alcoholicbeverages which are in an intermediate stage of aging with further agingto be carried out.

The aging period can be from 1 month to 30 years, or from 1 month to 24years, or from 1 month to 18 years, or from 1 month to 16 years, or fromone month to 14 years, or from 1 month to 12 years, or from 1 month to10 years, or from 1 month to 8 years, or from 1 month to 5 years, orfrom 1 month to 3 years, or from 1 month to 1 year, or from 1 month to 8months, or from 1 month to 6 months, or from 1 month to 4 months, orfrom 1 month to 3 months, or from 2 months to 15 years, or from 2 monthsto 6 years, or from 3 months to 12 years, or from 3 months to 5 years,or from 4 months to 12 years, or from 4 months to 14 months, or from 6months to 10 years, or from 6 months to 6 years, or from 6 months to 5years, or from 6 months to 1 year, or from 1 year to 8 years.

As used herein, the phrase “angels' share” refers to the amount ofalcoholic beverage lost to diffusion through a wooden barrel followed byevaporation into the atmosphere. The amount of alcoholic beverage lostincludes all ingredients of the beverage, e.g., water, ethanol, andother components.

During aging in some regions, in addition to the loss of ethanol, thereis also a concern for the loss of moisture from the barrel. However, thegreater concern is the loss of ethanol from the barrel. In tropicalclimates, the loss of ethanol can be high enough that the evaporativeloss is greater than the added value of the organoleptic characteracquired by the aging of the alcoholic beverage in the barrel.

Unless otherwise excluded in an above aspect or embodiment thereof, in afurther embodiment of any of the above aspects and embodiments, with thefilm covering at least 60% of the outer surface of the barrel, theangels' share can be reduced by at least 30%, or at least 40%, or atleast 50%, or at least 60%, relative to a control barrel containing acontrol alcoholic beverage aged without any film covering the controlbarrel the barrel. With the film surrounding the barrel, the angels'share loss can be reduced from 30% to 99.9%, or from 40% to 99%, or from50% to 98%, or from 60% to 97%, or from 70 to 97%, or from 74.3 to 96%,or from 82% to 95.5%, or from 89.4% to 95.5%, relative to a controlbarrel containing a control alcoholic beverage aged without any filmcovering the control barrel the barrel.

In assessing angels' share loss, and/or organoleptics (aroma, flavor,and/or color) of the subject aged alcoholic beverage (i.e., thealcoholic beverage aged in the barrel covered by or surrounded by thefilm) versus a control aged alcoholic beverage (i.e., alcoholic beverageaged in barrel not covered by film), the control barrel containing thecontrol alcoholic beverage is a barrel of the same size, composition,source, and condition as the subject barrel which is covered with thefilm in the aging of the alcoholic beverage. Moreover, the controlbarrel is filled with an alcoholic beverage identical to (e.g., takenfrom the same uniformly mixed batch) the alcoholic beverage in thesubject barrel. Finally, the aging conditions (temperature, humidity,etc) of the control alcoholic beverage are identical to the agingconditions alcoholic beverage in the subject barrel, e.g., samewarehouse, same ambient conditions.

Alternatively, during aging the wt % angels' share loss per year can befrom can be from 0.1 to 1.8 wt %, or from 0.2 to 1.5 wt %, or from 0.2to 1.3 wt %, or from 0.3 to 1.2 wt %.

The alcoholic beverage product can increase in proof level during aging.This may occur if the moisture vapor transmission rate (MVTR) of thefilm covering or surrounding the subject barrel is substantially higherthan the ethanol transmission rate (ETA) of the film covering orsurrounding the subject barrel.

Covering the barrel with the film can be carried out by placing thebarrel inside a bag made from the film. The bag can be closed with aclip, a heat seal, a zipper, a hook and loop closure, an adhesive, etc.The bag can be an end-seal bag, a side-seal bag, an L-seal bag, a pouch(i.e., U-seal bag), a backseamed bag (with a fin-type backseam or alap-type backseam).

FIG. 1 is a schematic of a preferred end-seal bag 10, in a lay-flatposition; FIG. 2 is a cross-sectional view of bag 10 taken throughsection 2-2 of FIG. 1. Viewing FIGS. 1 and 2 together, bag 10 comprisesbag film 11, top edge 12 defining an open top, first bag side edge 13,second bag side edge 14, bottom edge 15, and end seal 16.

FIGS. 3 and 4 illustrate side-seal bag 18. FIG. 3 illustrates aschematic of side seal bag 18, in a lay-flat view; FIG. 4 illustrates across-sectional view taken through section 4-4 of FIG. 3. With referenceto FIGS. 3 and 4 together, side seal bag 18 is comprised of bag film 19,top edge 20 defining an open top, bottom edge 21, first side seal 22,and second side seal 23.

FIG. 5 is a lay-flat view of a preferred L-seal bag 26, in a lay-flatposition. FIG. 6 is a transverse cross-sectional view of L-seal bag 26,taken through section 6-6 of FIG. 5. FIG. 7 is a longitudinalcross-sectional view of L-seal bag 26 taken through section 7-7 of FIG.5. Viewing FIGS. 5, 6, and 7 together, L-seal bag 26 has side-seal 28,bottom seal 30, open top 32, seamless folded bag side edge 34, andseamed bag side edge 36.

The fin-seal backseamed bag 38 of FIGS. 8 and 9 has open top 40, bottomseal 42, first folded side edge 44, second folded side edge 46, bottomedge 48, backseam seal 50 (inside film layer heat sealed to itself), andbackseam fins 52.

The lap-seal backseamed bag 54 of FIGS. 10 and 11 has open top 55,bottom seal 56, first folded side edge 58, second folded side edge 60,bottom edge 62, and backseam seal 64 (inside film layer heat sealed tooutside film layer).

FIGS. 12, 13, and 14 illustrate a pouch-type bag 66 made from sealingtwo separate pieces of flat film together. In FIGS. 12, 13, and 14,pouch 66 has open top 68, bottom heat seal 70 and bottom edge 72, firstside seal 74 and first side edge 76, second side seal 78 and second sideedge 80. Together, first and second side seals 74 and 76 connect withbottom seal 70 to form a “U-shaped” seal connecting the two pieces offlat film together to form the pouch-type bag 66.

FIG. 15 is a schematic of a process used to make a heat-shrinkable filmsuch as could be used to make a heat-shrinkable bag. The process of FIG.15 utilizes solid state orientation to produce polymer stress at atemperature below the melting point, whereby the resulting oriented filmis heat shrinkable. In the process illustrated in FIG. 15, solid polymerbeads (not illustrated) are fed to a plurality of extruders 80 (forsimplicity, only one extruder is illustrated). Inside extruders 80, thepolymer beads are forwarded, melted, and degassed, following which theresulting bubble-free melt is forwarded into die head 82, and extrudedthrough annular die, resulting in tubing 84 which is 5-40 mils thick,more preferably 20-30 mils thick, still more preferably, about 25 milsthick.

After cooling or quenching by water spray from cooling ring 86, tubing84 is collapsed by pinch rolls 88, and is thereafter fed throughirradiation vault 90 surrounded by shielding 92, where tubing 84 isirradiated with high energy electrons (i.e., ionizing radiation) fromiron core transformer accelerator 94. Tubing 84 is guided throughirradiation vault 90 on rolls 96. Preferably, the irradiation of tubing84 is at a level of about 7 MR.

After irradiation, irradiated tubing 98 is directed over guide roll 100,after which irradiated tubing 98 passes into hot water bath tank 102containing water 104. The now collapsed irradiated tubing 98 issubmersed in the hot water for a retention time of at least about 5seconds, i.e., for a time period in order to bring the film up to thedesired temperature, following which supplemental heating means (notillustrated) including a plurality of steam rolls around whichirradiated tubing 98 is partially wound, and optional hot air blowers,elevate the temperature of irradiated tubing 98 to a desired orientationtemperature of from about 240° F. to about 250° F. Thereafter,irradiated film 98 is directed through nip rolls 106, and bubble 108 isblown, thereby transversely stretching irradiated tubing 98.Furthermore, while being blown, i.e., transversely stretched, irradiatedfilm 98 is drawn (i.e., in the longitudinal direction) between nip rolls106 and nip rolls 114, as nip rolls 114 have a higher surface speed thanthe surface speed of nip rolls 106. As a result of the transversestretching and longitudinal drawing, irradiated, biaxially-oriented,blown tubing film 110 is produced, this blown tubing preferably havingbeen both stretched at a ratio of from about 1:1.5-1:6, and drawn at aratio of from about 1:1.5-1:6. More preferably, the stretching anddrawing are each performed at a ratio of from about 1:2-1:4. The resultis a biaxial orientation of from about 1:2.25-1:36, more preferably,1:4-1:16.

While bubble 108 is maintained between pinch rolls 106 and 114, blowntubing 110 is collapsed by rolls 112, and thereafter conveyed throughnip rolls 114 and across guide roll 116, and then rolled onto wind-uproll 118. Idler roll 120 assures a good wind-up.

FIG. 16 illustrates a schematic view of a process for making a non-heatshrinkable film, i.e., a “hot-blown” film, which is oriented in the meltstate and is not heat shrinkable. Although only one extruder 139 isillustrated in FIG. 16, there can be more extruders, such as 2 or 3extruders. Extruder 130 supplies molten polymer to annular die 131 forthe formation of the film, which can be monolayer or multilayer,depending upon the design of the die and the arrangement of theextruder(s) relative to the die, as known to those of skill in the art.Extruder 130 is supplied with polymer pellets suitable for the formationof the film. Extruder 130 subjects the polymer pellets to sufficientheat and pressure to melt the polymer and forward the molten streamthrough die 131.

Extruder 130 is equipped with screen pack 132, breaker plate 133, andheaters 134. The film is extruded between mandrel 135 and die 131, withthe resulting extrudate being cooled by cool air from air ring 136. Themolten extrudate is immediately blown into blown bubble 137, forming amelt oriented film. The melt oriented film cools and solidifies as it isforwarded upward along the length of bubble 137. After solidification,the film tubing passes through guide rolls 138 and is collapsed intolay-flat configuration by nip rolls 139. The collapsed film tubing isoptionally passed over treater bar 140, and thereafter over idler rolls141, then around dancer roll 142 which imparts tension control tocollapsed film tubing 143, after which the collapsed film tubing iswound up as roll 144 via winder 145.

FIG. 17 is a schematic of a packaged alcoholic beverage product 150. InFIG. 17, which has barrel 152 within a bag that has been sealed closed.Barrel 152 is made from staves 154 held together by hoops 155 and hastop 157 and bottom (not illustrated). Barrel 152 is covered by bag 156having top edge 158, top heat seal 160, bottom edge 162, and bottom heatseal 164.

EXAMPLES

The present invention can be further understood by reference to thefollowing examples that are merely illustrative and are not to beinterpreted as a limitation to the scope of the present invention thatis defined by the appended claims. The films of the examples containedvarious resins identified in the table below.

Tradename/ Supplier Chemical Nature Acronym Properties & Parameterst50-200-178 High density polyethylene HDPE-1 0.952 g/cm³ Ineos 2.0 g/10min Surpass ® EX-HPs667 AB01 High density polyethylene HDPE-2 0.967g/cm³ Nova Chemicals 6.0 g/10 min Surpass ® EX-HPs 167AB High densitypolyethylene HDPE-3 0.966 g/cm³ Nova Chemicals 1.2 g/10 min T60-500-119High density polyethylene HDPE-4 0.961 g/cm³ Ineos 6.2 g/10 min Dowlex ®2037 Medium Density Polyethylene MDPE 0.935 g/cm³ Dow (Ziegler nattacatalyzed) 2.5 g/10 min Dowlex ® 2045.04 Linear Low Density PolyethyleneLLDPE-1 0.920 g/cm³ Dow (Ziegler natta catalyzed) 1.0 g/10 min Dowlex ®2045.03 Linear Low Density Polyethylene LLDPE-2 0.920 g/cm³ Dow (Zieglernatta catalyzed) 1.1 g/10 min 6.5 wt % octene mer LDPE-662I Low DensityPolyethylene LDPE-1 0.919 g/cm³ Dow 0.47 g/10 min Escorene ® LD-200.48Low Density Polyethylene LDPE-2 0.915 g/cm³ ExxonMobil 7.5 g/10 min EB403AQ Low Density Polyethylene LDPE-3 0.924 g/cm³ Westlake Chemical 0.8g/10 min Elite ® 5400G Polyethylene, Linear Low Density ssc EAO-1 0.917g/cm³ Dow Ethylene/Octene Copolymer - 1.1 g/10 min Single Site/SingleSite Affinity ® PL 1840G Polyethylene, Very Low Density ssc EAO-2 0.9090g/cm³ Dow Ethylene/Octene Copolymer - 1.0 g/10 min Branched, Single SiteExceed ® 4518 Single site catalyzed ssc EAO-3 0.918 g/cm³ ExxonMobilethylene/hexene copolymer 4.5 g/10 min Affinity ® EG 8100G Single sitecatalyzed ssc EAO-4 0.870 g/cm³ Dow ethylene/octene copolymer 0.99 g/10min Exceed ® 1012 CA Single site catalyzed ssc EAO-5 0.912 g/cm³ExxonMobil Linear low density polyethylene 1.0 g/10 min Exceed ® 1012HASingle site catalyzed ssc EAO-6 0.912 g/cm³ ExxonMobil Linear lowdensity polyethylene 1.0 g/10 min Wintec WFW4F Single site catalyzed sscEAO-7 0.90 g/cm³ Japan Polypropylene propylene/ethylene copolymer 7.0g/10 min Affinity PL 1850G Single site catalyzed ethylene ssc EAO-80.902 g/cm³ Dow octene copolymer 3.0 g/10 min Exact ® 3128 Single sitecatalyzed ssc EAO-8 0.900 g/cm³ ExxonMobil Very low density polyethylene1.2 g/10 min Fortron ® PPS FX4382T1 Ethylene/octene block copolymerEAO-BC 1.264 g/cm³ EOD-01-03 Propylene-ethylene copolymer PEC 0.90 g/cm³Total Petrochemical 8.0 g/10 min Surlyn ® AM7927 Zinc NeutralizedEthylene Ion 0.980 g/cm³ DuPont Methacrylic Acid copolymer 11.5 g/10 minSurlyn ® 1859 Zinc Neutralized Ethylene Ion-2 0.94 g/cm³ DuPontMethacrylic Acid copolymer 4.0 g/10 min EF437AA Ethylene/vinyl acetatecopolymer EVA-1 0.925 g/cm3 Westlake Chemical 2.0 g/10 min 2.5 wt %vinyl acetate LD319.32 Ethylene/vinyl acetate copolymer EVA-2 0.930 g/ccExxonMobil 2.0 g/10 min Petrothene ® NA 340013 Ethylene/vinyl acetatecopolymer EVA-3 0.924 g/cc LyondellBasell Ind 1.0 g/10 min Plexar ® PX3227 Maleic anyhydride modified m-LLDPE-1 0.913 g/cm³ Nippon GosheiLLDPE 1.7 g/10 min Plexar ® PX3610X01 Maleic Anhydride-Modifiedm-LLDPE-2 0.918 g/cm³ Lyondell Basell Ind. Polyethylene, Linear LowDensity 2.1 g/10 min Plexar ® PX 3410 Maleic Anhydride-Modified Linearm-LLDPE-3 0.918 g/cm³ Lyondell Basell Ind. Low Density polyethylene 1.1g/10 min Plexar ® PX 3236 Maleic Anhydride-Modified Linear m-LLDPE-40.921 g/cm³ Lyondell Basell Ind. Low Density polyethylene 2.0 g/10 minNF 539A Anhydride modified linear low m-LLDPE-5 0.91 g/cc MitsuiChemical density polyethylene 1.7 g/10 min Plexar ® PX 2246 MaleicAnhydride-Modified High m-HDPE-1 0.95 g/cm³ Lyondell Basell Ind. Densitypolyethylene 0.63 g/10 min Plexar ® PX 2220 Maleic Anhydride-ModifiedHigh m-HDPE-2 0.943 g/cm³ Lyondell Basell Ind. Density polyethylene 5.5g/10 min E171B Hydrolyzed ethylene vinyl acetate EVOH1 1.14 g/cm³Evalca/Kuraray copolymer 1.7 g/10 min 44 mol % ethylene Soarnol ®SGN017B Hydrolyzed Ethylene/Vinyl Acetate EVOH2 1.2 g/cm³ Nippon GohseiCopolymer, Lubricated - Less than 3.8 g/10 min 30 mole % Ethylene 27.5mol % ethylene Grilon ® CF6S Polyamide 6/12 PA6/12 Density 1.05 g/cm³,EMS-Grivory Melt Index 5.75 g/10 min (Cond. 230° C./2.16 kg), MeltingPoint 130° C. Ultramid ® B40 LN01 Polyamide - 6, Lubricated and PA6 1.14g/cm³ BASF Nucleated - Poly(caprolactam) melt point 220° C. Ultramid ®B40 Polyamide - 6 PA6-2 1.13 g/cm³ BASF (polycaprolactam) melt point230° C. Ultramid ® C33 01 Polyamide 6/66 PA6/66 1.13 g/cm³ BASF 196° C.melt point Ultramid C40 L01 Polyamide 6/66 PA6/66-2 1.125 g/cc BASF 190°C. melt point MXD6 Nylon S6007 Polyamide MXD6 PA-MXD6 0.122 g/ccMitsubishi Engineering - 237° C. melt point Plastics Eastar PETG 6763Polyethylene terephthalate glycol PETG 1.27 g/cm³ Eastman Chemical 2.8g/10 min Eastapak Copolyester 9921 Copolyester CO-PET 1.40 g/cm³ EastmanChemical 255° C. melt point G1645MO styrene ethylene butene terpolymerSEB 0.885 g/cm³ Kraton Polymers 3.25 g/10 min Topas ® 8007 F-04 Ethylenenorbornene copolymer ENB-1 1.02 g/cm³ Topas Advanced Polymers, Inc. 32g/10 min 36 mol % norbornene Topas ® 9903D-10 Ethylene/NorborneneCopolymer ENB-2 0.974 g/cm³ Topas Advanced Polymers, Inc. 1.0 g/10 minTopas ® 8007F-400 Ethylene/Norbornene Copolymer ENB-3 1.02 g/cm³ TopasAdvanced Polymers, Inc. 2.04 g/10 min Topas ® E-140 Cyclic OlefinCopolymer ENB-4 0.94 g/cm³ Topas Advanced Polymers, Inc. 3.0 g/10 minKemester ® 300 Special Mixed Glycerol Fatty Acid AF 0.96 g/c³ PMCBiogenics Ester/Propylene Glycol antifog agent Polybutylene-1 PB 8640MButene/ethylene copolymer PB 0.90 g/cm³ LyondellBasell Industries(polybutylene) 1 g/10 min High Purity Ethyl Acetate ethyl acetate HPEthAcet 0.9015 Eastman Chemical Adcote 842 Solvent based PolyurethanePUAdh-1 — Rohm and Haas CR 842B adhesive Aliphatic isocyanate, polyol,ethyl PuAdh-2 — Rohm and Haas acetate Kemamide ® E Ultra Bead eurcamidewax WAX-1 0.8150 g/cm³ PMC-Biogenix 81° C. melt point Kemamide ® W-40Prill N,N′-ethylene-bis stearamide wax WAX-2 0.995 g/cm³ PMC-Biogenix146° C. melt point Kemamide ® VO amide-oleamide wax WAX-3 0.920 g/cm³PMC-Biogenix 73° C. melt point Kemamide ® B Bead amide wax-behenamideWAX-4 0.8070 g/cm³ PMC-Biogenix Kaopolite ® SF Anhydrous aluminumsilicate AB-1 2.62 g/cm³ Kaopolite, Inc Antiblocking agent 1% moisture502835 Sodium Calcium Aluminosilicate AB-2 1.06 g/cm³ Ampacet and Talcin High Density 4.8 g/10 min Polyethylene Superfine Super FlossSilica-calcined diatomaceous AB-3 2.3 g/cm³ Celite earth LP 102.74Antiblock and slip in low density AB-4 0.920 g/cm³ ExxonMobilpolyethylene 6.5 g/10 min 10622 Antiblock in low density polyethyleneAB-5 0.92 g/cc Ampacet FSU 255E Slip and antiblock in polyethyleneS&AB-1 1.08 g/cm³ Schulman 8.0 g/10 min 100458 Fluoropolymer in LLDPE:PA-1 0.93 g/cm³ Ampacet Processing aid 1.4 g/10 min 102804 Antiblock andslip in high density AB/S 1.02 g/cc Ampacet polyethylene 7.1 g/10 min95% EVA-1 Polymer blend PolyBlnd see components 3.3% WAX-2 above 1.7%AB-3 90.8% EVA-1 Masterbatch MB see components 3.4% WAX-1 above 3.3%WAX-2 1.7% AB-3 0.8% WAX-3

Example 1 Comparative

A first set of ninety-eight empty, used American standard white oakcasks were each overwrapped (i.e., “bagged”) using an end-seal bag madefrom transparent, heat-shrinkable Film No. 1, described below. Eachwooden cask had a length of 100 centimeters and a maximum diameter of 55centimeters. The bag placed over each cask was an end-seal bag having alay-flat width of 115 cm and a length of 200 cm. Each empty cask waspackaged by standing the cask upright on end, with the open end of theend-seal bag dropped down over the upright cask until the end-sealcontacted the top of the cask. The cask was then inverted while the bagwas held in place around the cask. After inverting the cask 180 degrees,i.e., other end up, the open end of the bag was pulled upward and theexcess bag length was gathered together over the upper cask end.Pressure-sensitive packaging tape (equivalent or similar to Scotch® 3750Commercial Performance packaging tape) was wrapped around the gatheredexcess bag length immediately over the upper end of the cask, therebyenclosing the cask inside the bag and effectively enveloping the caskwithin the bag.

After bagging the cask, the bung hole in the cask was visually locatedthrough the transparent film. A small piece of the bag film (i.e., 2.5to 3.5 cm in diameter) was cut away, exposing the bung hole. Using thepassageway through the bung hole, the cask was then filled with maltdistillate from a dip tank and a bung was driven into the bung hole toseal the cask closed. No film patch was secured over the hole cut intothe film over the bung hole.

Using an air gun, the bags around the first ten of the ninety-eightcasks were shrunk before the bagged casks were filled and transported toand placed on the aging rack. During the shrinking of the bag film onthe first ten casks, it was noticed that the film strained along thesteel hoops, and caused the film to tear in the vicinity of the hoopswhile the film was shrinking. Moreover, during transport of theresulting bagged casks, the shrunken film exhibited significant tearingduring transport to the aging rack. After racking ten of theninety-eight casks, it was decided not to shrink the film against theeleventh cask, and it was found that the film over the eleventh caskexhibited less tearing during transport than the films that were shrunkaround the casks. As a result, the bag film was not shrunken for theremaining eighty-seven casks.

Each of the first set of ninety-eight bagged, filled casks weretransported from the bagging and filling area to the storage rack in thedistillate aging warehouse. During the transport of the bagged casks,the bags suffered damage, including numerous holes and tears on thestaves and in the hoop areas as the casks were rolled and otherwisemoved onto a storage rack for aging of the alcoholic beverage, with theshrunken films exhibiting more holes and tears than the unshrunkenfilms.

The rack was present in a warehouse in which outdoor temperatures rangedfrom about 12° C. to 30° C. in the winter, and from about 22° C. to 40°C. in the summer. The first set of ninety-eight bagged casks were loadedonto the same distillate aging rack, which had a capacity of about 115casks. The first set of ninety-eight bagged, filled casks were placed onthe rack.

The first set of bagged casks remained on the rack, unmoved, for aperiod of one year. After the year of aging on the rack, the agedalcoholic beverage in each of the first set of ninety-eight casks waspoured into an empty dip tank, with the volume and ethanol content ofthe aged alcoholic beverage measured and compared against the initialvolume and initial ethanol content of the malt distillate alcoholicbeverage. Moreover, the aged alcoholic beverage was tested fororganoleptic properties.

A second set of ninety-eight empty American standard used white oakcasks, each also having a volume of 53 gallons and filled with the samemalt spirit from the same batch of distillate from the same dip tank,was aged during the same year as the first set of bagged casks was aged.The oak casks of the second set were not bagged, and were left withoutany overwrap and aged as comparative examples. The second set ofninety-eight unbagged, comparative casks were racked on another similarrack in the same warehouse, and as with the first set of casks. The agedalcoholic beverage from the second set of ninety-eight unbagged caskswas also emptied into an empty dip tank, with the volume, ethanolcontent, and organoleptic properties of the aged alcoholic beverage fromthe unbagged casks measured and compared against the initial volume andinitial ethanol content of the malt distillate alcoholic beverage placedinto the unbagged casks.

The results of the tests obtained for the aged alcoholic beverage fromninety-eight aged, bagged casks were compared against the test resultsobtained for the ninety-eight aged, unbagged casks.

Film No. 1, had the following layer arrangement and layer composition:

Film No. 1 Layer 1 Layer 8 (inside) Layer 2 Layer 3 Layer 4 Layer 5Layer 6 Layer 7 (outside) 71% LLDPE mLLDPE-1 80% PA 6/66 EVOH1 90% EVOH180% PA 6/66 mLLDPE-1 71% LLDPE 24% MDPE 20% Ion 10% PA 6/12 20% Ion 24%MPDE 4% AF 4% AF 1% AB-1 1% AB-1 (0.27 mil) (0.09 mil) (0.09 mil) (0.09mil) (0.09 mil) (0.09 mil) (0.09 mil) (0.27 mil)

Film No. 1 was a heat-shrinkable, heat-sealable film multilayer filmhaving eight layers and a total thickness of 1 mil before shrinking.Layer 4 contained saponified ethylene/vinyl acetate copolymer (alsoreferred to as “ethylene/vinyl alcohol copolymer”) having a thickness of0.09 mm. Layer 4 controlled the oxygen transmission rate of the entirefilm because it had the lowest OTR of any of the film layers. Film No. 1also had outer ethylene-based layers providing heat sealability andabuse resistance.

Each end-seal bag was made by heat sealing across a seamless extrudedtubing having a lay-flat width of 115 centimeters. After the end-sealwas made, the inside layer of the multilayer tubing film was heat sealedto itself at intervals of 200 centimeters. The tubing was cuttransversely about 1 cm below the transverse heat seal, to produce theend-seal bags. Heat-shrinkable Film No. 1 was produced using a processas illustrated in FIG. 15, described above. The end-seal bag was asillustrated in FIGS. 1 and 2, described above.

On a bulk liter basis, the results demonstrated that the 1 mil thickFilm No. 1 reduced the loss from 12.84% for the unbagged casks to 10.52%for the bagged casks, which is an 18.07% reduction in diffusion andevaporation loss on a bulk liter basis. Since the 18.07% reduction inbulk liter loss was greater than the 16.2% reduction in proof literloss, it is apparent that while the bagging of the casks in Film No. 1reduced the loss of both water and ethanol from the cask, the baggingreduced the loss of water more than the loss of ethanol, i.e., the bagwas somewhat more of a barrier to the moisture vapor than to theethanol.

After the 12 months of aging, sensory testing (i.e., taste testing) ofthe aged distillate revealed no noticeable difference between theorganoleptic properties of the distillates in the bagged casks versusthe organoleptic properties of the distillate in the unbaggedcomparative casks. It was recognized that the numerous holes and tearscould have contributed to the migration of enough atmospheric oxygenthrough the cask walls and into the distillate to enable the oxidativereactions that result in the formation of desired organolepticcomponents such as esters, etc. Thus, the holes and tears could havebeen partially or wholly responsible for the result that the ageddistillate had an organolepic character equivalent to the unbaggedcomparative casks.

The discovery that the 16.2% reduction in Angels' Share proof-liter lossof Example 1 occurred even though the bags had numerous holes and tearsduring the 12 month aging period, led to the conception that a moreeffective reduction in Angels' Share proof-liter loss could be effectedif the bags of Film No. 1 were overwrapped with a second bag made from atough film. This conception was the basis for the design of Example 2,below.

Example 2 Comparative

A set of ten used American standard used white oak casks, each having avolume of 53 gallons, were filled with malt spirit from a dip tank. Thecasks themselves were identical to the casks utilized in Example 1. Eachcask was “double bagged” by being first bagged in a bag made fromtransparent, heat-shrinkable transparent Film No. 1 (described above),the bags being identical to the bags used in Example 1. The resultingbagged cask was bagged again (i.e., “overbagged” or “double bagged”) byhaving a second bag made from transparent Film No. 2 placed over thecask and over the bag made from Film No. 1.

After placing both bags over the cask, the open end of both bags werepulled upward and the excess bag length was gathered together over theupper cask end. As with the bagged casks of Example 1,pressure-sensitive packaging tape was wrapped around the gathered excessbag lengths immediately over the upper end of the cask, therebyenclosing the cask inside the first bag, while simultaneously enclosingboth the cask and first bag in inside the second bag.

A set of ten control casks were also prepared using the same type ofbarrels and using the same malt spirit from the same dip tank. However,the ten control casks were left to age without coverage by any film,i.e., with the cask surface in direct contact with the ambientenvironment in the aging warehouse.

Film No, 2, had the following layer arrangement and layer composition.

Film No. 2 Layer 1 (inside) Layer 2 Layer 3 50% LLDPE-2 90% LLDPE-2 50%LLDPE-2 25% MDPE 4.5% LLDPE 25% MDPE 24.6% EVA 3.4% C₃/C₂ copolymer24.6% EVA 0.26% WAX-2 2% polypropylene 0.26% WAX-2 0.14% AB-3 0.5%polybutylene 0.14% AB-3 (0.53 mil) (1.94 mils) (0.53 mil)

As with Film No, 1, Film No. 2 was also heat-shrinkable andheat-sealable. Film No. 2 was a multilayer film having three layers anda total thickness of 3 mils before shrinking. Film No. 2 was madeprimarily from ethylene-based polymers. Film No. 2 was thick and tough,providing abuse-resistance in an effort to prevent the formation ofholes and tears during transport of the casks from the bagging area tothe aging rack. However, Film No. 2 did not contain an O₂-barrier layer.Film No. 2 was also produced using a process as illustrated in FIG. 15,described above.

The bagged casks remained on the rack, unmoved, for a period of sixmonths. The control casks were aged on a similar rack at a similar levelin the warehouse. When the malt spirit was added to each of the twentycasks (i.e., the ten casks of the example plus the ten control casks),the average volume of the malt spirit in each cask was 200.25 liters.After the six months of aging, the average volume in each of the tendouble bagged casks was 187 liters, while the average volume in each ofthe ten double bagged casks was 181 liters. Thus, the bagged caskssuffered an average fluid loss of 13.25 liters (i.e., 6.6%), while theunbagged control casks suffered an average fluid loss of 19.25 liters(i.e., about 9.6%). The use of the doubled bags around the ten casks ofexample 2 reduced the fluid loss level about 3.3% of the 9.6% fluid lossthat occurred for the ten unbagged control casks, i.e., approximately a34.4% reduction in the level of fluid loss.

In addition, a blind taste test was conducted of the aged malt spritfrom the ten bagged casks versus the aged malt spirit from the tenunbagged control casks. The perception of the taste tester was that theliquid from the wrapped casks possessed “smoother notes” than the liquidfrom the unwrapped casks. Moreover, the liquid from the wrapped caskswas marginally darker in color versus the liquid from the control casks.

Additional films have been prepared for use in the preparation of apackaged alcoholic beverage product. Several of these films contained anethylene/norbornene copolymer. It has been found thatethylene/norbornene copolymer can be used to make a film providing thecombination of (i) a relatively low ethanol transmission rate, (ii) arelatively low water vapor transmission rates, and while at the sametime providing (iii) a relatively high O₂ transmission rate.

Film No. 3 through Film No. 16, set forth below, can be used to make apackaged alcoholic beverage product, with the package being suitable foraging. In a single package, the films can be used either singly or oneon top of another. The alcoholic beverage can be placed in a woodenbarrel which is thereafter sealed closed and then partially covered orfully covered with the film. Supplemental films such as the relativelythick and abuse resistant Film No. 2, described above, can be usedovertop of any one or more of Film Nos. 2 through Film No. 16.

Film No. 3 Layer 1 Layer 7 (inside) Layer 2 Layer 3 Layer 4 Layer 5Layer 6 (outside) 22% LDPE-1 mLLDPE-2 PA6 EVOH2 PA6 mLLDPE-2 60% ENB-170% LLDPE 15% HDPE-1 8% AB-2 20% ssc-LLDPE 5% AB-2 (1.93 mils) (0.28mil) (0.55 mil) (0.55 mil) (0.55 mil) (1.10 mils) (0.55 mil)

Film No. 4 Layer 1 Layer 6 (inside) Layer 2 Layer 3 Layer 4 Layer 5(outside) 74% LLDPE 45% LLDPE ENB-2 LLDPE 45% LLDPE 74% LLDPE 22.74% EVA40% ssc EAO-2 (0.06 mil) (0.06 mil) 40% ssc EAO-2 22.74% EVA 1.17% WAX-113.8% EVA 13.8% EVA 1.17% WAX-1 0.91% WAX-2 0.45% WAX-1 0.45% WAX-10.91% WAX-2 0.86% AB-1 0.27% WAX-2 0.27% WAX-2 0.86% AB-1 0.32% AB-30.14% WAX-3 0.14% WAX-3 0.32% AB-3 (0.04 mil) 0.30% AB-1 0.30% AB-1(0.04 mil) (0.05 mil) (0.05 mil)

Film No. 5 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 ssc EAO-3 ssc EAO-4ssc HDPE-2 ssc EAO-4 ssc EAO-3 (0.4 mil) (0.6 mil) (1.0 mil) (0.6 mil)(0.4 mil)

Film No. 6 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 ssc EAO-3 ssc EAO-4ssc HDPE-3 ssc EAO-4 ssc EAO-3 (0.4 mil) (0.6 mil) (1.0 mil) (0.6 mil)(0.4 mil)

Film No. 7 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 70% ssc EAO-3 sscEAO-4 EAO-5 ssc EAO-4 70% ssc EAO-3 30% AB-4 (0.6 mil) (1.0 mil) (0.6mil) 30% AB-4 (0.4 mil) (0.4 mil)

Film No. 8 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 70% ssc ssc 70% ENB-3ssc 70% ssc EAO-3 EAO-4 30% ssc EAO-4 EAO-3 30% AB-4 (0.6 mil) EAO-5(0.6 mil) 30% AB-4 (0.4 mil) (1.0 mil) (0.4 mil)

Film No. 10 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 70% ssc ssc 70%ENB-3 ssc 70% ssc EAO-3 EAO-4 30% ssc EAO-4 EAO-3 30% AB-4 (0.6 mil)EAO-5 (0.6 mil) 30% AB-4 (0.4 mil) (1.0 mil) (0.4 mil)

Film No. 11 Layer 1 Layer 2 Layer 3 EVA-2 60% ENB-3 HDPE-4 20% PB 40%EAO-5 (0.4 mil) 2% AB-5 (3.2 mils) (0.4 mil)

Film No. 12 Layer 1 Layer 2 Layer 3 EVA-2 70% ENB-3 HDPE-4 20% PB 30%EAO-5 (0.4 mil) 2% AB-5 (3.2 mils) (0.4 mil)

Film No. 13 Layer 1 Layer 2 Layer 3 EVA-2 80% ENB-3 HDPE-4 20% PB 20%EAO-5 (0.4 mil) 2% AB-5 (3.2 mils) (0.4 mil)

Film No. 14 Layer 1 Layer 2 Layer 3 98% LUNG 30% ENB-3 98% EVA-3 2% AB-570% ssc EAO-5 2% AB-5 (0.9 mil) (2.7 mils) (0.9 mil)

Film No. 15 100% ENB-3 (4 mils; cast monolayer film)

Film No. 16 was made from 100% cyclic olefin copolymer and exhibited anethanol transmission rate of 0.0175 g/m²/day, an oxygen (O₂)transmission rate (“OTR”) of 50 cc g/m²/day, and a moisture vaportransmission rate (“MVTR”) of 0.078 g/m²/day.

Film No. 16 Layer 1 (monolayer film) 100% Fortron ® PPS FX 4382T1polyphenylene sulfide (6 mils; cast film)

Weight Loss Studies of Pouches Made from Films 17-22

Film Numbers 17-22, set forth below, were prepared. Film Nos. 17, 18,and 19 were hot blown (i.e., not heat shrinkable) films prepared inaccordance with the process illustrated in FIG. 16, described above.Film Nos. 20, 21, and 22 were oriented (i.e., heat-shrinkable) filmsmade in accordance with the process illustrated in FIG. 15, describedabove.

Below is a table providing a summary of cyclic olefin copolymer contentand total film gauge for each of Film Nos. 17-22. For each of Film Nos.17-22, more detailed information is present in Tables 20 through 25,below.

Solid State Oriented Wt % COC Wt % COC Film No. or Hot Blown (in blendin layer) (total film basis) 22 SS Oriented 0 0 21 SS Oriented 50 12.520 SS Oriented 70 18.25 17 Hot Blown 0 0 18 Hot Blown 50 30 19 Hot Blown70 49

Each of Film Nos. 17-22 was used to make a plurality of pouches thatwere filled with various liquids and sealed closed to make a packagedproduct. The packaged products were place in conditioned storage forspecified periods, and were periodically removed for a brief period sothat the weight of the packaged product could be measured.

Each of Film Nos. 17-22 was tested using each of three different fluids.A first fluid, termed a “duplicating fluid,” contained “95%ethanol”+anhydrous esters. More particularly, the duplicating fluid wasDuplicating Fluid no. 5, i.e., DPF 501, obtained from SolvChem, Inc. DPF501 contained 85-90% ethanol (CAS #64-17-5) [European EC #200-578-6],0-10% n-propyl acetate (CAS #109-60-4), and 0-5% isopropanol (CAS#67-63-0) [European EC #200-661-7]. The second fluid was a 60 vol %/40vol % (52 wt %/47 wt %) mixture of ethanol and water. The third fluidwas 100% water.

For each of Film Nos. 17-22, a first set of five pouches packaging thefirst fluid (DPF 501) were stored at 32° C. and 40% relative humidity. Asecond set of five pouches packaging DPF 501 were stored at 32 C and 70%relative humidity. A first set of five pouches containing the secondfluid (60/40 ethanol/water mix) were stored at 32° C. and 70% relativehumidity. A second set of five pouches containing the second fluid werestored at 32° C. and 40% relative humidity. A first set of five pouchescontaining the third fluid (100% water) were stored at 32° C. and 70%relative humidity. A second set of five pouches containing the thirdfluid (100% water) were stored at 32° C. and 40% relative humidity.Thus, in the weight loss tests, a total of 180 pouches were tested,i.e., thirty pouches for each of the six films tested.

The change in weight provided evidence of the permeability of the filmas a function of the film layer arrangement, layer composition, andlayer thickness, the type of liquid contained in the package, and theambient conditions during storage, i.e., the temperature and relativehumidity. In this manner, each of Film Nos. 17-22 were assessed forweight change as a function of type of solution in the pouch, ambientconditions in which the pouch was stored, and length of time in thepouch.

The ratio of surface area of American standard oak barrels (53 gallon)to weight of distillate inside the barrel was calculated as 5643 in² for53 gallons having a density of 0.89 (i.e., a fluid weight of 178,557grams), producing a surface area (SA) to weight (g) ratio of 5643 in² to178,557 grams=0.031 in²/g. The ratio of surface area of 5 gallon oaktest barrels to weight of distillate inside the test barrel wascalculated 1465 in² containing 5 gallons liquid (16,845 grams),resulting in a surface area to weight ratio of 1465 in² to 16,845 gramsof 0.086 in²/g.

The packaged products made up using the 180 pouches provided from about8× to about 11× greater surface area to weight ratio than the barrelsurface area to distillate weight values calculated values above. Eachpackaged product was made from a single piece of film six inches longand four inches wide. It was folded in half and sealed along each sideedge, resulting in a pouch having lay-flat dimensions of 4 inches wideand 3 inches long, with an appearance substantially corresponding withthe side-seal bag of FIGS. 3 and 4, described above. The ratio ofsurface area of the pouch to weight of liquid inside the pouch wascalculated as follows. For 100% water, the inside surface area wasassumed to be 24 in², and 100 grams of water were place in the pouch,producing a surface area to weight ratio of 24 in²/100 g, =0.24 in²/g,which is about 8× the SA/g of the American standard barrel. For the60/40 ethanol/water blend, the inside surface area was assumed to be 24in², and 80 grams of the blend were place in the pouch, producing asurface area to weight ratio of 24 in²/80 g, =0.30 in²/g, which is about10× the SAIg of the American standard barrel. For the pouches filledwith DPF501, the inside surface area was assumed to be 24 in², and 70grams of the blend were place in the pouch, producing a surface area toweight ratio of 24 in²/70 g, =0.34 in²/g, which is about 11× the SAIg ofthe American standard barrel. In this manner, the higher surface areaper gram of fluid provided the potential to accelerate the relativeamount of weight change of the liquid in the pouch, relative to theamount of weight change likely to occur with a standard oak barrelsurrounded by the same film.

FIGS. 19-24 are graphical representations of the data obtained from theweight loss studies of the 180 pouches. FIG. 19 provides the testresults for Film No. 22. FIG. 20 provides the test results for Film No.21. FIG. 21 provides the test results for Film No. 20. FIG. 22 providesthe test results for Film No. 17. FIG. 23 provides the test results forFilm No. 18. FIG. 24 provides the test results for Film No. 19.

As can be seen in FIGS. 19-24, the rate of weight loss varied as afunction of the nature of the liquid, the conditions of storage, and thetype of film. Films with the highest amount of cyclic olefin copolymer(Film Nos. 19 and 20, containing 49% and 18.25% cyclic olefin copolymer,respectively) exhibited the lowest rates of weight loss (0.48% and 0.8%loss of water, respectively, at 40% relative humidity) compared withfilms containing less cyclic olefin copolymer, and in fact exhibitedweight gain in samples containing DPF501. In contrast, films with thelowest amount of cyclic olefin copolymer (Film Nos. 17 and 22, each with0% cyclic olefin copolymer) exhibited the highest rates of weight losscompared with the films containing more cyclic olefin copolymer, and infact respectively exhibited 14% and 11% weight loss in the samplescontaining DPF501 at 40% relative humidity. The two films containing theintermediate levels of cyclic olefin copolymer (Film Nos. 18 and 21)produced intermediate results with respect to weight loss.

The data in FIGS. 19-24 is rearranged in FIGS. 25-27. FIG. 25 is a plotof weight loss as a function of time for all of the samples containingthe DPF501 liquid, and reveals that Film No. 17, which was a hot blownfilm, exhibited a higher rate of weight loss than Film No. 22, which wasa solid state oriented (i.e., heat shrinkable) film. FIG. 25 also showsthat all the films containing the cyclic olefin copolymer actuallyincreased in weight as a function of time, rather than losing weight.

FIG. 26 is a plot of weight loss as a function of time for all of thepouches containing 100% water. FIG. 26 revealed that the greater thefilm thickness and the greater the amount of cyclic olefin copolymer,the lower the rate of water lost from the pouch.

FIG. 27 is a plot of weight loss as a function of time for all of thepouches containing the 60/40 blend of ethanol and water. As pointed outabove, the films possessing 0% cyclic olefin copolymer exhibited thehighest rate of weight loss, while the films exhibiting the lowest rateof weight loss contained the highest percentage of cyclic olefincopolymer.

FIG. 28 is a plot of weight loss as a function of time forpouch-in-pouch arrangements wherein the innermost pouch was in each casemade from Film No. 22 (containing 0% cyclic olefin copolymer) filledwith DPF501 fluid. Three samples were overpouched with the same Film No.22, containing 0% cyclic olefin copolymer. One pouch was large (foldeddimensions 6 inches by 8 inches), one pouch was medium sized (foldeddimensions 4.5 inches by 6.5 inches) and one pouch was small (i.e.,“snug) with folded dimensions of 3.5 inches by 5 inches. The other halfof the inner pouches were overpouched with Film No. 20, which contained18.25% cyclic olefin copolymer, with the same three sizes of overpouchesused, i.e., 6″×8″, 4.5″×6.5″, and 3.5″×5″. As shown in FIG. 28, thepouch-in-pouch results utilizing the outer pouch containing 18.25%cyclic olefin copolymer exhibited lower rates of weight loss than thepouch-in-pouch results utilizing the outer pouch containing 0% cyclicolefin copolymer. Moreover, the snug pouch-in-pouch samples having snugouter pouches exhibited lower rate of weight loss than the correspondingsamples having large outer pouches.

Distillate Aging in Small Casks Enveloped in Films 17-20 and 22-25

Film Numbers 17-25, set forth below, were prepared. Film Nos. 17, 18, 19and 23 were hot blown (i.e., not heat shrinkable) films prepared inaccordance with the process illustrated in FIG. 16, described above.Film Nos. 20, 21, 22, 24, and 25 were oriented (i.e., heat-shrinkable)films made in accordance with the process illustrated in FIG. 15,described above. Several large bags were made from each of Film Nos.17-20 and 22-25. Inside each bag was placed an oak barrel (53 gallons)filled with a distillate liquid. For each of Film Nos. 17-20 and 22-25,three or four distillate-filled barrels were packaged in a bag, with thebagged barrels being placed on a rack for aging of the distillate.

Film No. 17 Layer 1 Layer 2 Layer 3 70% sscEAO-3 sscEAO-6 70% sscEAO-330% LDPE-2 (2.10 mils) 30% LDPE-2 (0.45 mil) (0.45 mil)

Film No. 18 Layer 1 Layer 2 Layer 3 70% sscEAO-3 50% sscEAO-6 70%sscEAO-3 30% LDPE-2 50% ENB-3 30% LDPE-2 (0.45 mil) (2.10 mils) (0.45mil)

Film No. 19 Layer 1 Layer 2 Layer 3 70% sscEAO-3 30% sscEAO-6 70%sscEAO-3 30% LDPE-2 70% ENB-3 30% LDPE-2 (0.45 mil) (2.10 mils) (0.45mil)

Film No. 20 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 50% LLDPE-2 LLDPE-270% ENB-3 LLDPE-2 50% LLDPE-2 25% MDPE (0.34 mil) 30% ssc (0.34 mil) 25%MDPE 17% EVA-1 EAO-6 17% EVA-1 8% PolyBlnd (0.64 mil) 8% PolyBlnd (0.34mil) (0.34 mil)

Film No. 21 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 50% LLDPE-2 LLDPE-250% ENB-3 LLDPE-2 50% LLDPE-2 25% MDPE (0.34 mil) 50% ssc (0.34 mil) 25%MDPE 17% EVA-1 EAO-6 17% EVA-1 8% PolyBlnd (0.64 mil) 8% PolyBlnd (0.34mil) (0.34 mil)

Film No. 22 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 50% LLDPE-2 LLDPE-2LLDPE-2 LLDPE-2 50% LLDPE-2 25% MDPE (0.34 mil) (0.64 mil) (0.34 mil)25% MDPE 17% EVA-1 17% EVA-1 8% PolyBlnd 8% PolyBlnd (0.34 mil) (0.34mil)

Film No. 23 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 sscEAO-5 m-LLDPE-4EAO-BC m-LLDPE-4 sscEAO-5 (0.70 mil) (0.30 mil) (1.0 mil) (0.30 mil)(0.70 mil)

Film No. 24 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 92% LLDPE-1 LLDPE-150% ENB-3 LLDPE-1 92% LLDPE-1 8% MB (0.50 mil) 50% sscEAO-6 (0.50 mil)8% MB (0.25 mil) (1.00 mil) (0.25 mil)

Film No. 25 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 92% LLDPE-1 LLDPE-170% ENB-3 LLDPE-1 92% LLDPE-1 8% MB (0.50 mil) 30% sscEAO-6 (0.50 mil)8% MB (0.25 mil) (1.00 mil) (0.25 mil)

Film No. 26 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 50% LLDPE-2 LLDPE-2ssc EAO-6 LLDPE-2 50% LLDPE-2 25% MDPE (0.34 mil) (0.64 mil) (0.34 mil)25% MDPE 17% EVA-1 17% EVA-1 8% PolyBlnd 8% PolyBlnd (0.34 mil) (0.34mil)

Film No. 27 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 50% LLDPE-2 LLDPE-260% ENB-3 LLDPE-2 50% LLDPE-2 25% MDPE (0.34 mil) 40% ssc (0.34 mil) 25%MDPE 17% EVA-1 EAO-6 17% EVA-1 8% PolyBlnd (0.64 mil) 8% PolyBlnd (0.34mil) (0.34 mil)

Film No. 28 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 92% LLDPE-1 LLDPE-160% ENB-3 LLDPE-1 92% LLDPE-1 8% MB (0.50 mil) 40% sscEAO-6 (0.50 mil)8% MB (0.25 mil) (1.00 mil) (0.25 mil)

Film No. 29 Layer 1 Layer 2 Layer 3 70% sscEAO-3 50% sscEAO-6 70% HDPE-430% LDPE-2 50% ENB-3 30% LDPE-2 (0.45 mil) (2.10 mils) (0.45 mil)

Film No. 30 Layer 1 Layer 2 Layer 3 70% sscEAO-3 40% sscEAO-6 70%sscEAO-3 30% LDPE-2 60% ENB-3 30% LDPE-2 (0.45 mil) (2.10 mils) (0.45mil)

Film No. 31 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 70% sscEAO-3sscEAO-4 20% sscEAO-6 sscEAO-4 70% sscEAO-3 30% AB-4 (0.6 mil) 80% ENB-3(0.6 mil) 30% AB-4 (0.4 mil) (1.0 mil) (0.4 mil)

Film No. 32 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 sscEAO-5 m-LLDPE-475% EAO-BC m-LLDPE-4 sscEAO-5 (0.70 mil) (0.30 mil) 25% ENB-3 (0.30 mil)(0.70 mil) (1.0 mil)

Film No. 33 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 sscEAO-5 m-LLDPE-450% EAO-BC m-LLDPE-4 sscEAO-5 (0.70 mil) (0.30 mil) 50% ENB-3 (0.30 mil)(0.70 mil) (1.0 mil)

Film No. 34 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 70% ssc EAO-4 sscEAO-4 ENB-3 ssc EAO-4 ENB-4 30% SEB (2.0 mils) (0.5 mil) (2.0 mils) (0.8mil) (0.7 mil)

Film No. 35 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 70% ssc EAO-4 sscEAO-4 ENB-4 ssc EAO-4 ENB-4 30% SEB (2.0 mils) (0.5 mil) (2.0 mils) (0.8mil) (0.7 mil)

Various films above exhibited the following properties:

Ratio Ratio ETR OTR MVTR Energy OTR OTR Film (g/100μ/ (cc/m²/ (g/100in²/Peak Load to Break to to No. m²/day) day) day) (Newtons) (Joules) ETRMVTR 15 0.0178 200 0.02 — — 11,236 10,000 1 1.6 40 1.2 75 0.55 25 33.313 0.266 325 0.44 91 0.5 1222 739 12 380 0.055 123 1.25 — 6,909 110.0375 390 0.064 130 1.5 10,400 6,094 14 0.9565 1275 0.18 117 2.67 13297,083 16 0.04845 128 0.35 136 1.8 2642 366 2 — 3300 0.65 200 1.8 — 5,07734 0.373 1750 0.29 67 1.22 4692 6,034 35 5.69 2900 0.45 77 3.09 5106,444

Additional films were prepared or obtained, as follows:

Film No. 36 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 Layer 6 Layer 7 PETGCO-PET CO-PET CO-PET 85% CO-PET CO-PET CO-PET 15% PA-MXD6 (0.28 mil)(0.28 mil) (0.28 mil) (0.08 mil) (0.28 mil) (0.27 mil) (0.09 mil)

Film No. 37 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 47% LLDPE-1 67%m-EBC 90 67% m-EBC 47% LLDPE-1 23.5% EVA1 33% EVOH-1 33% 23.5% EVA123.5% MDPE LLDPE-2 10 PA6/12 LLDPE-2 23.5% MDPE 4% AF (0.27 mils) (0.13mil) (0.27 mils) 4% AF 2% WAX 4 2% WAX 4 (0.27 mil) (0.27 mil)

Film No. 37 exhibited a modulus of 95,000 psi in each of thelongitudinal direction and the transverse direction.

Film No. 38 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 98% EVA-3 70% EAO-670% EAO-6 70% EAO-6 98% EVA-3 2% AB-5 30% ENB-3 30% ENB-3 30% ENB-3 2%AB-5 (0.9 mil) (0.67 mils) (1.35 mil) (0.67 mils) (0.9 mil)

Film No. 39 Monolayer film made from 100% PVC

Film No. 40 polyethylene Metal foil Ionomer resin

This film was SP Class PPD Barrier Packaging Film obtained from ShieldPack Specialty Packaging. It had a total thickness of 3.9 mils and anOTR of less than 0.003 cc/100 in²/day and a WVTR of less than 0.003g/100M²/day. It was four layer structure having the following layerarrangement:

Film No. 41 Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 9-layer 53.33% BOPET53.33% 5-layer Laminate PUAdh-1 (0.52 mil) PUAdh-1 Laminate (see below)42.67% EtAcet 42.67% EtAcet (see below) (2.75 mils) 4% PUAdh-2 4%PUAdh-2 (1.00 mil) (0.18 mils) (0.18 mils)

In Film No. 41, BOPET was a biaxially oriented polyester film, coatedwith an acrylic bonder on one side. BOPET was obtained from Kureha. Ithad a thickness of 0.52 mil and a density of 1.4 g/cc.

9-Layer Laminate in Film No. 41

Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 Layer 6 Layer 7 Layer 8 Layer 950% PEC 60% MHD-1 Ion-2 PA6-2 mLLDPE-5 PA6-2 PA6/66-2 mLLDPE-5 50% PEC44% sscEAO-9 40% MHD-2 44% sscEAO-9 6% AB/S 6% AB/S 0.64 mil 0.17 mil.14 mil 0.28 mil 0.22 mil .28 mil 0.18 mil 0.39 mil 0.46 mil

5-Layer Laminate in Film No. 41

Layer 1 Layer 2 Layer 3 Layer 4 Layer 5 50% PEC mLLDPE-5 PA6-2 mLLDPE-550% PEC 49% sscEAO-9 0.18 mil 0.25 mil 0.18 mil 49% sscEAO-9 1% AB/S 1%AB/S 0.23 mil 0.17 mil

Film No. 42 Layer 1 Layer 2 Layer 3 Layer 4 50% ssc EAO-8 60% sscEAO-6LLDPE-1 70% sscEAO-5 48% LDPE-2 40 ENB-3 (0.07 mil) 28% LLDPE-3 2%S&AB-1 (0.42 mils) 2% PA-1 (0.14 mil) (0.27 mils)

Angels' Share Weight Loss Test No. 1 Shrink-Wrapped and Vacuum-PackagedBarrels Vs Control

All barrels were pre-soaked with water for hydration for 2-10 days. Whenthe barrel swelled and met the saturation point the barrel wasconsidered to be ready to fill with 60% duplicating fluid 5 anhydrous(Lot No. 82013826198) and 40% water. The barrels were then wrapped withthe films described below. The barrels were stored in an indoor cabinetand weighed weekly. This test was conducted following the protocol andprocedures previously mentioned.

Four 1-liter control barrels were not wrapped. Four 1-liter barrels wereshrink-wrapped in Film No. 36. Four 1-liter barrels were shrink-wrappedin Film No. 22. Four 1-liter barrels were vacuum-packaged in Film No.19. Four 1-liter barrels were shrink-wrapped in Film No. 25. Two 3-literbarrels were shrink-wrapped in Film No. 25. Two 5-liter barrels wereshrink-wrapped in Film No. 25. The shrink-wrapped and vacuum-packagedbarrels were allowed to age for 45 days. The average percentage weightloss for each treatment was calculated.

Percent Weight Loss after 45 Days

Barrel Barrel Volume Total Average Sample Identity Treatment (liters)Weight Loss (%) Control Unwrapped 1 9.92 Film No 36 Shrink-wrapped 10.88 Film No. 22 Shrink-wrapped 1 0.53 Film No. 19 Vacuum-packaged 10.31 Film No. 25 Vacuum-packaged 1 0.13 Film No. 25 Shrink-wrapped 30.17 Film No. 25 Shrink-wrapped 5 0.23

As is apparent from the data in the table above, the control barrel lostsignificantly more weight (angels' share) than all the treatment wrappedbarrels. All of the treatment wrapped barrels had statistically similarangels' share reduction when stored over 45 days

Angels' Share Weight Loss Test No. 2 Shrink-Sleeve, Shrink-Bag, andLoose-Bag Packaged Barrels Vs Control

All barrels were pre-soaked, saturated, wrapped, and stored as in weightloss test No. 1, above. Test 2 consisted of 24 barrels: four 1-literbarrels shrink-sleeve packaged in Film No. 36; four 1-liter barrelsshrink-sleeve packaged in Film No. 25; four 1-liter barrels shrink bagpackaged in Film No. 25; four 1-liter barrels loose bag packaged in FilmNo. 25; two 3-liter unwrapped control barrels; two 5-liter unwrappedcontrol barrels; four 1-liter unwrapped control barrels. This test wasconducted for 42 days (1-liter barrels) and 45 days for (3 L or 5 Lbarrels), and the average percentage weight loss for each treatment wascalculated.

Percent Weight Loss after 42 Days (1-Liter Barrels) 45 Days (3 & 5-LiterBarrels)

Barrel Barrel Volume Total Average Sample Identity Treatment (liters)Weight Loss (%) Control Unwrapped 1 5.35 Film No. 36 Shrink-Sleeve 16.32 Film No. 25 Shrink-sleeve 1 7.12 Film No. 25 Shrink- bag 1 0.02Film No. 25 Loose-bag 1 0.00 Control Unwrapped 3 11.44 Control Unwrapped5 7.23

The barrels shrink bag packaged in Film No. 25 and loose-bag packaged inFilm No. 25 had a significant reduction in angels' share compared withthe control barrels. However, the barrels shrink-sleeve packaged in FilmNo. 36 and Film No. 25 did not have a significant reduction in angels'share compared with the control barrels.

Angels' Share Weight Loss Test No. 3 Pallet-Wrapped, 2″-Wrapped, and6″-Wrapped Packaged Barrels Vs Control

All barrels were pre-soaked, saturated, wrapped, and stored as in weightloss test No. 1, above. Test 3 consisted of 20 barrels: four 1-literunwrapped control barrels; four 1-liter barrels individually stretchedwrapped with 6-inch film strips with barrels on pallet, using Film No.25; four 1-liter barrels with barrels and pallet wrapped together as onepackage, using a bag made from Film No. 25; four 1-liter barrelsindividually wrapped with 2″ wide film strips using Film No. 25 (butfilm having 0.75 mil total thickness, wrapped three times to obtain 2.25mils total film thickness); four 1-liter barrels stretch wrapped with 2″strips of Film No. 25 (but at 1.1 mil total thickness). The test wasconducted for 49 days and the average percentage weight loss for eachtreatment was calculated.

Barrel Volume Total Average Barrel Treatment (liters) Weight Loss (%)Control (unwrapped) 1 11.87 Pallet 1 (four barrels) 11.31 Film No. 25(Pallet wrapped in bag) 1 (four barrels) 0.24 Film No. 25: 6″ strips(Pallet) 1 (four barrels) 16.52 A1 2″ strips (0.75 mil) 1 6.14 4C 2″strips (1.1 mil) 1 5.18

Barrels wrapped in treatments A1 2″ strips (0.75 mil), Film No. 25pallet wrapped in bag and 4C 2″ strips (1.1 mil) demonstratedsignificant reduction in “angel share” compared to the controlbarrels/control pallet. However, the barrels wrapped in Film No. 25 6″strips had a statistically significant increase in “angel share”compared to the controls. Film No. 25 pallet wrapped bag had thegreatest reduction in “angel share” and it was statistically differentfrom all other treatments.

Angels' Share Weight Loss Test No. 4 Pallet-Wrapped, 2″-Wrapped, and6″-Wrapped Packaged Barrels vs Control

All barrels were pre-soaked, saturated, wrapped, and stored as in weightloss test No. 1, above. Barrel test 4 consisted of 24 barrels: Four 1 Lbarrels packaged in Film No. 19 (packaged in a bag); four 1 L barrelspackaged in Film No. 41 1.1 mil (2″ strips wrapped); four 1 L barrelspackaged in Film No. 42 0.7 mil (2″ strips wrapped); four 1 L barrelspackaged in Film No. 42 1.1 mil (2″ strips wrapped); one 3 L barrelspackaged in Film No. 42 1.1 mil (3″ strip wrapped); one 5 L barrelpackaged in Film No. 42 1.1 mil (2″ strip wrapped); four 1 L controlbarrels (not wrapped); one 3 L control barrel (not wrapped) and one 5 Lbarrel (not wrapped). All barrels had the ends of the barrel left open.The barrels were wrapped to achieve and approximate 2.2 mil thicknessonce wrapped. This test was conducted following the protocol andprocedures previously mentioned. This test was conducted for 49 days andthe average percentage weight loss for each treatment was calculated.

Barrel Volume Normalized Barrel Treatment (liters) Weight Loss (%) FilmNo. 19 (bag) 1 0.00 Film No. 41 2″ strips (1.1 mil) 1  6.08. Film No. 422″ strips (0.7 mil) 1 12.08  Film No. 42 2″ strips (1.1 mil) 1 7.51 FilmNo. 42 3″ strips (1.1 mil) 3 3.5  Film No. 42 3″ strips (1.1 mil) 5 1.94Control (unwrapped) 1 7.60 Control (unwrapped) 3 7.64 Control(unwrapped) 5 5.40

Angels' Share Weight Loss Test No. 5 COC-Wrapped, Foil-Wrapped,Barrier-Film, PVC-Wrapped Packaged Barrels vs Control

All barrels were pre-soaked, saturated, wrapped, and stored as in weightloss test No. 1, above. Barrel test 5 used virgin wheat whiskey in 10barrels. Two barrels were packaged in Film No. 19, two barrels werepackaged in foil based Film No. 40, two barrels were packaged in PVCFilm No. 39, and two control barrels not wrapped were utilized. Weightswere measured on day 0 and day 49. The test demonstrated the outcomewhen oxidation is unable to occur during maturation. Sensory testing wasconducted on various samples.

Barrel Barrel Volume Total Average Treatment (liters) Weight Loss (%)Control 1 15.22 (unwrapped) NFX4672 (bag) 1 0.11 Film No. 40 (Foil) 10.04 Film No. 39 (PVC) 1 1.54

Sensory Consumer Taste Panel Test No. 1

Three triangle tests were conducted in order to evaluate if a differencein color, aroma or taste exists between (i) grain neutral spirit (GNS)samples aged in control barrels (unwrapped), and (ii) GNS samples agedin barrels wrapped in Film No. 19, or (iii) GNS samples aged in barrelswrapped in Film No. 16, or (iv) GNS samples aged in barrels wrapped inFilm No. 1.

The ONS was 190 proof (USP/NF grade) derived solely from corn, procuredfrom Pharmco Products Inc. The GNS was proofed down to 60% using reverseosmosis treated H₂O and used to fill 5 gallon new oak barrels.

Preference information was also requested for the samples in thistriangle test, as well as the additional triangle tests disclosed below.However, the preference responses were incomplete and were deemed not tobe statistically significant.

The barrels were 5-gallon new oak barrels charred on the inside. Thesamples were aged for 249 days. All barrels were aged in the samewarehouse environment.

The barrels (control, and barrels aged while wrapped in Film Nos. 19,17, and 1) were weighed prior to sampling. The barrels were agitated forthree minutes each using a four wheel dolly. Barrels were vented androtated at half the agitation time. All samples were collected using acommercially sterile method and all equipment was cleaned and sanitizedprior to use.

Separate equipment was used for each sample to prevent crosscontamination between samples. Samples were stored in glass jars withparaffin wrapped around the closure. Jars were placed in foil bags toprevent both oxygen and light from entering. 800 Milliliters of GNS wascollected from each barrel: 100 milliliters for proof testing, 500milliliters for sensory testing and 200 milliliters for analyticaltesting. Proof testing was conducted using a Mettler Toledo No. AD-1260(China), with Alcodens Version 2.5 analytical program. The warehousetemperature was 50° F. during sampling. Analytical testing samples werestored in amber vials with paraffin wrapped around the closure.

The GNS samples submitted for analytical testing were analyzed todetermine whether there was a difference in compounds developed duringmaturation between the four samples. The analytical data determined thatall the compounds sought were present in each GNS sample. The GNS samplefrom the barrel wrapped in Film No. 1 had a higher concentration ofguaiacol, conferaldehyde and syringol but otherwise contained a similarprofile.

The consumer panel testing was carried out in accordance with theStandard Guide for Sensory Evaluation of Beverages Containing AlcoholASTM E1879-00, which is hereby incorporated, in its entirety, byreference thereto. There were a total of 16 consumer panelists. Thepanel was a convenient sample of typical consumers. A presentationexplaining general sensory practices was provided to the panel membersprior to conducting Panel Test No. 1.

The hypothesis tested was whether consumer panelists were capable ofdetecting an organoleptic difference between the control sample (from anunwrapped barrel) versus the samples from barrels wrapped in Film No 19,Film No. 17, and Film No. 1. Panelists detected a difference between theControl sample and the sample from the barrel wrapped in Film No. 1. Themajor difference between the Control and the sample from the barrelwrapped in Film No 1 was color (the control sample was lighter),followed by differences in taste and aroma.

The hypothesis was rejected for the other two triangle tests as thepanelists were not able to detect a difference between the controlsample (from an unwrapped barrel) and the samples from barrels wrappedin Film No 19 and Film No. 17.

Due to high sample alcohol by volume (ABV) of greater than 57%, andconcerns of overwhelming the panelist's senses, the samples were diluted50/50 using demineralized water, in accordance with ASTM E1879-00,yielding an ABV of about 30%. All samples were stored at roomtemperature and color coded with tissue paper to prevent panelist biasduring pouring. All samples were served in 1 ounce plastic vials withthe clarity of glass. Panelists were provided with unsalted crackers andwater to cleanse their palates. In addition, spit cups were provided.

Each triangle test had separate evaluation sheets with different samplecodes. All codes were randomly selected and assigned to treatments. Eachpanelist was also assigned a number, and the serving order of the threetriangle tests was randomized.

The panelists were asked to evaluate the color of the product first,followed by aroma and finally, taste. The panelists were then asked toselect the different sample. Follow-up information was also requested:(a) how different was the sample: mark on a scale of weak to verystrong; (b) why was the sample different (color, aroma, taste or all ofthe above); and (c) whether the panelists preferred the different sample(yes or no).

Triangle Test 1 consisted of three samples: two samples of GNS from thebarrel wrapped in Film No. 19 (49 wt % cyclic olefin copolymer), and onecontrol sample (barrel not wrapped). This test was conducted followingthe protocol and procedures above.

Triangle Test 2 consisted of three samples: two samples of GNS from thebarrel wrapped in Film No. 17 (0% COC) and one control sample (barrelnot wrapped). This test was conducted following the protocol andprocedures above.

Triangle Test 3 consisted of three samples: two samples of GNS from thebarrel wrapped in Film No. 1 (containing EV OH oxygen barrier layer) andone control sample (barrel not wrapped). This test was conductedfollowing the protocol and procedures above.

The table below summarizes the parameters measured before collectingsamples for analytical testing and sensory testing. Each barrel wasweighed prior to aging (initial weight), and then after aging (finalweight) but before agitation. Initial samples were then collected forproof measurements, where the temperature was monitored.

Angels' Share Weight Loss after about 10 Months of Aging in 5-Gallon OakBarrels

Average Average Average Average Barrel Initial Final Weight PercentageTreatment weight (kg) weight (kg) Loss (kg) Weight Loss Control 30.9125.60 1.32 4.26 (unwrapped) Film No. 19 31.08 31.00 0.08 0.26 Film No.17 30.79 30.53 0.26 0.84 Film No. 1 30.95 30.59 0.36 1.16

Results of Triangle Test 1 (aged GNS from Control barrel vs. aged GNSfrom barrel surrounded by Film No. 19): the hypothesis was rejectedbecause less than 10 panelists selected the correct different sample.Only seven panelists were able to detect a difference.

Results of Triangle Test 2 (aged GNS from Control barrel vs. aged GNSfrom barrel surrounded by Film No. 17): the hypothesis was rejectedbecause less than 10 panelists selected the correct different sample.Only five panelists were able to detect a difference.

Results of Triangle Test 3(aged GNS from Control barrel vs. aged GNSfrom barrel surrounded by Film No. 1): the hypothesis was acceptedbecause at least 10 panelists selected the correct different sample.Eleven panelists were able to detect a difference.

Triangle Test Results from Consumer Panel Test No. 1

Detectable difference of taste, aroma, and color Triangle compared tothe Temperature Test No. Treatment control Proof (° F.) — Control N/A118.90 55.22 (unwrapped) 1 Control vs. Film NO (7/16)* 114.66 57.80 No.19 2 Control vs. Film NO (5/16)* 115.14 57.60 No. 17 3 Control vs. FilmYES (11/16)* 114.70 57.70 No. 37 *For a statistically significantdifference of p = 0.05 between samples and acceptance of the hypothesis,a minimum of 10 of the 16 panelist need to detect a difference byselecting the correct “different” sample (Meilgaard, Civille and Carr,Sensory Evaluation Techniques, 3^(rd) Ed., CRC Press LLC, 1991, which ishereby incorporated in its entirety, by reference thereto; seeparticularly page 369)

ph for Each Barrel and Comments Provided from Analytical Lab

Treatment pH value Comments Control 4.42 Sweet, light in color Barrelwith Film No. 19 4.07 Sweet, light in color Barrel with Film No. 17 3.95Sweet, light in color Barrel with Film No. 37 3.98 Phenolic (bad smell),dark color

The analytical lab tested for the presence of each of the followingcompounds: vanillin, eugenol, syringaldehyde, guaiacol, cresol isomers,coniferaldehyde, syringol, 4-methylguaiacol, and methyl octalactones. Inattempting to correlate the sensory data with the analytical data theresearchers searched for difference in the aged distillate from thebarrel covered by Film No. 1, compared to the other three samples(Control, Film #19, and Film #17). The analytical data revealed that allthe compounds were present in each of the four GNS samples. The GNSsample from the barrel covered by Film No. 1 had a higher concentrationof guaiacol, coniferaldehyde and syringol, but otherwise contained asimilar profile. Guaiacol is extracted from the lignin and produces inthe oak from which the barrel is made, and provides a “smoky” aroma andflavor. If present in too high of a concentration it can lead to“off-flavors.”

It is hypothesized that the panelists could differentiate the ageddistillate from the barrel covered by Film No. 1 because of the colordifference between this aged distillate and the Control. The sample fromthe barrel covered by Film No. 1 had a darker color than the Control.The color formation during maturation is linked to the content of gallicacid and ellagic acid (water soluble tannins) in the aged distillate.These compounds also lead to astringency in GNS sample. These compoundscan later be oxidized to give fragrant compounds. The sample from thebarrel covered by Film No. 1 had the greatest oxygen barrier (i.e.,lowest oxygen transmission rate) relative to the Control, Film No. 19,and Film No. 17, and could have prevented these compounds from beingoxidized. pH readings were in the range of 3.95 (barrel surrounded byFilm No. 17) to 4.42 (Control).

The following conclusions were drawn from the results of Panel Test No.1 and analytical analysis of the samples: (1) the aged GNS from thebarrel covered by Film No. 1 had significantly different organolepticproperties compared to the control sample by sensory testing methods;(2) the consumer taste panelists were not able to detect a differencebetween the GNS aged in the Control (unwrapped barrel) and the GNS agedin the barrel surrounded by Film No. 19, or the difference between theGNS aged in the Control (unwrapped barrel) and the GNS aged in thebarrel surrounded by Film No. 17; and (3) GNS aged in Film No. 1 had adarker color than the other samples and greater production of guaiacol,coniferaldehyde and syringol.

Sensory Consumer Taste Panel Test No. 2

Three triangle tests were conducted in order to evaluate if a differencein color, aroma or taste exists between grain neutral spirit (GNS)samples aged in new 5-gallon oak control barrels (unwrapped), versus (i)GNS samples aged in new 5-gallon oak barrels wrapped in Film No. 20, orversus (ii) GNS samples aged in barrels wrapped in Film No. 22, orversus (iii) GNS samples aged in new 5-gallon oak barrels wrapped inFilm No. 16. The hypothesis tested was whether consumer panelists werecapable of detecting an organoleptic difference between the controlsample (from the unwrapped barrel) and the samples from barrels wrappedin Film No. 20, Film No. 22, or Film No. 16. A difference was detectedby the panelists between all wrapped barrel samples and the controlsample. The major difference was color (the control sample was lighter)followed by differences in taste and aroma.

The barrels were 5-gallon new oak barrels charred on the inside. Thesamples were aged for 249 days. All barrels were aged in the samewarehouse environment. The four barrels (control, and barrels aged whilewrapped in Film Nos. 20, 22, and 16) were weighed prior to sampling, andthe barrels were agitated, vented, rotated, and samples collected as inPanel Test No. 1, above. The equipment used, sample storage, and takingof sample volumes was also performed as in Panel Test No. 1, above. Thewarehouse temperature was 58° F. during sampling. Analytical testingsamples were stored in amber vials with paraffin wrapped around theclosure.

The results of the analytical testing determined that all the compoundswere present in each GNS sample. The Control GNS (unwrapped) always hadthe lowest concentration of each compound. The GNS packaged in Film #22had the highest concentration of every compound except: hexose,guaiacol, syringol, and guaiacyl acetone.

The samples were tested for the presence of the following compounds:vanillin, eugenol, syringaldehyde, guaiacol, cresol isomers,coniferaldehyde, syringol, 4-methylguaiacol, s-hydroxymethyl furan,pyrogallol, sinapinaldehyde, methoxy eugenol, acetosyringone, benzoicacid, methyl homovanillate, syringic acid, 4-methyl guaiacol, 4-methylsyringol, 4-vinyl guaiacol, hexadecanoic acid, octadecanoic acid,ellagic acid, o-trimethyl ellagic acid, quercetin(2-(3,4-dihydroxyphenyl)-3,5,7-trihydroxy-4H-chromen-4-one, furfural(2-furanaldehyde), whiskey lactone, 5-furancarboxaldehyde, guaiacylacetone, hexose, beta-d-glucopyranose, and methyloctalactones. Thesamples were also tested for pH.

In attempting to correlate the sensory data with the analytical data theresearchers searched for a difference in the packaged barrel samplescompared to the control (unpackaged GNS). The analytical data determinedthat all the compounds were present in each GNS sample. The unpackedcontrol GNS sample always had lowest concentration of each compound. GNSpackaged in NFX 2131 had the highest concentration of every compoundexcept: hexose, guaiacol, syringol, furfural, whiskey lactone,5-furancarboxaldehyde and guaiacyl acetone (which it had similar amountsto the other treatments). GNS packaged in PPS was high in furfural,whiskey lactone and 5-furancarboxaldehyde. GNS packaged in NFX2133 washigh in hexose, syringol and guaiacyl acetone.

It was hypothesized that the panelist could differentiate the packagedbarrel samples from the control mainly due to color differences. Thepackaged samples had a darker color. The color formation duringmaturation is linked with the gallic acid and ellagic acid (watersoluble tannins). The tannins decompose during charring/toasting oraging the process, oxygen penetrates into the whiskey through the barrelwood and oxidizes solutes. Whiskey tannins are generated by opening upthe pyrogallol attached to glucose.

The Standard Guide for Sensory Evaluation of Beverages ContainingAlcohol ASTM E1879-00 was used for conducting Panel Test No. 2. Thepanel was a convenient sample of typical consumers. A presentationexplaining general sensory practices was provided to the panel membersprior to conducting Panel Test No. 2.

Due to high sample alcohol by volume (ABV) of greater than 57%, andconcerns of overwhelming the panelist's senses, the samples were diluted50/50 using demineralized water, in accordance with ASTM E1879-00,yielding an ABV of about 30%. All samples were stored at roomtemperature and color coded with tissue paper to prevent panelist biasduring pouring. All samples were served in 1 ounce plastic vials withthe clarity of glass. Panelists were provided with unsalted crackers andwater to cleanse their palates. In addition, spit cups were provided.Each triangle test had separate evaluation sheets with different samplecodes. All codes were randomly selected and assigned to treatments. Eachpanelist was also assigned a number, and the serving order of the threetriangle tests was randomized.

The panelists were asked to evaluate the color of the product first,followed by aroma and finally, taste. The panelists were then asked toselect the different sample. Follow-up information was also requested:(a) how different was the sample: mark on a scale of weak to verystrong; (b) why was the sample different (color, aroma, taste or all ofthe above); and (c) whether the panelists preferred the different sample(yes or no).

Triangle Test 1 consisted of three samples: two samples of aged GNS frombarrel surrounded by Film No. 16 (100% polyphenylene sulfide film,loose, uncompromised wrap) and one aged GNS sample from the Controlbarrel (barrel not wrapped). This test was conducted following theprotocol and procedures above.

Triangle Test 2 consisted of three samples: two samples of aged GNS frombarrel surrounded by Film No. 22 (0% COC, tight with heat shrink wrap)and one control sample (barrel not wrapped). This test was conductedfollowing the protocol and procedures above.

Triangle Test 3 consisted of three samples: two samples of GNS from thebarrel wrapped in Film No. 20 (18% COC, tight with heat shrink wrap) andone control sample (barrel not wrapped). This test was conductedfollowing the protocol and procedures above.

The table below summarizes the parameters measured before collectingsamples for analytical testing and sensory testing. Each barrel wasweighted prior to agitation and initial samples were, then collected forproof measurements, where the temperature was monitored.

Barrel Treatment Weights and Percentage “Angel Share” Lost

Average Average Average Average Barrel Initial Final Weight PercentageTreatment weight (kg) weight (kg) Loss (kg) Weight Loss Control 30.9125.60 1.32 4.26 (unwrapped) Film No. 20 30.58 30.46 0.12 0.39 Film No.22 30.95 30.78 0.17 0.54 Film No. 16 31.22 30.83 0.39 1.27The consumer taste panel had twenty six panelists. For a significantdifference of p=0.05 between samples and acceptance of the hypothesis, aminimum of 10 panelist need to detect a difference by selecting thecorrect “different” sample (Meilgaard, Civille and Carr, 1991)

Results of Triangle Test 1 (aged GNS from Control barrel vs. aged GNSfrom barrel surrounded by Film No. 20): The hypothesis can be acceptedbecause more than 14 panelists selected the correct different sample.Twenty panelists were able to detect a difference. The major differencewas color (the control sample was lighter) followed by differences intaste and aroma.

Results of Triangle Test 2 (aged GNS from Control barrel vs. aged GNSfrom barrel surrounded by Film No. 22): The hypothesis can be acceptedbecause more than 14 panelists selected the correct different sample.Fifteen panelists were able to detect a difference. The major differencewas color (the control sample was lighter) followed by differences intaste and aroma.

Results of Triangle Test 3 (aged GNS from Control barrel vs. aged GNSfrom barrel surrounded by Film No. 16): The hypothesis can be acceptedbecause more than 14 panelists selected the correct different sample.Twenty-one panelists were able to detect a difference. The majordifference was color (the control sample was lighter) followed bydifferences in taste and aroma.

Triangle Test Results from Consumer Panel Test No. 2

Triangle Taste, Aroma, Color Test No. Treatment Difference vs Control —Control Unwrapped N/A 1 Control vs. Film No. 20 YES (21/26)* (18% COC) 2Control vs. Film No. 22 YES (15/26)* (0% COC) 3 Control vs. Film No. 16YES (20/26)* (100% PPS) *Source Meilgaard, Civille and Carr (1991)

The following conclusions were drawn from the results of Panel Test No.2: (1) the GNS packaged all had significantly different organolepticproperties compared to the control sample. (2) some of consumer tastepanelists preferred the GNS stored in the packaging treatments barrelscompared to the control samples (unwrapped barrels).

Sensory Consumer Taste Panel Test No. 3

As described above, it was surmised that the color difference betweenthe control and the aged GNS Film Nos. 16, 20, and 22 enabled thepanelists in Panel Test No. 2 to determine the identity of the Controlsample (unwrapped), i.e., simply because the Control sample was lighterin color than the aged distillate samples taken from barrels covered byFilm Nos. 16, 20, and 22. As a result, in Panel Test No. 3, a new panelrepeated Panel Test No. 2. As there was enough aged distillate remainingafter the completion of Panel Test No. 2, the aged distillate used inPanel Test No. 3 was taken from the glass containers used to supply andstore the aged distillate used in Panel Test No. 2. However, in PanelTest No. 3 black cups were used to remove the color bias during thefirst three triangle tests which involved only aroma and taste, with theconsumer panel conducting three further and separate triangle tests,using clear cups, to evaluate only the color.

Thus, six triangle tests were conducted. The samples taken for sensorytesting in Panel Test No. 2 included enough extra GNS from each of thebarrels to conduct the six triangle tests of Panel Test No. 3. Exceptfor the use of the black cups in the first three triangle tests in PanelTest No. 3, the procedure used was the same as in Panel Test No. 2. Thepanel test was conducted as before, i.e., in accordance with TheStandard Guide for Sensory Evaluation of Beverages Containing AlcoholASTM E1879-00.

Triangle Test 1 consisted of three samples: two samples of aged GNS frombarrel surrounded by Film No. 16 (100% polyphenylene sulfide film,loose, uncompromised wrap) and one aged GNS sample from the Controlbarrel (barrel not wrapped). This test was conducted in black cupsevaluating only taste and smell. Otherwise, this test was conductedfollowing the protocol and procedures above.

Triangle Test 2 consisted of three samples: two samples of aged GNS frombarrel surrounded by Film No. 22 (0% COC, tight with heat shrink wrap)and one control sample (barrel not wrapped). This test was alsoconducted in black cups evaluating only taste and smell. Otherwise, thistest was conducted following the protocol and procedures above.

Triangle Test 3 consisted of three samples: two samples of GNS from thebarrel wrapped in Film No. 20 (18% COC, tight with heat shrink wrap) andone control sample (barrel not wrapped). This test was also conducted inblack cups evaluating only taste and smell. Otherwise, this test wasconducted following the protocol and procedures above.

Triangle Test 4 consisted of three samples: two samples of aged GNS frombarrel surrounded by Film No. 16 (100% polyphenylene sulfide film,loose, uncompromised wrap) and one aged GNS sample from the Controlbarrel (barrel not wrapped). This test was conducted in clear cups, andthe panelists were instructed to evaluate color only. Otherwise, thistest was conducted following the protocol and procedures above.

Triangle Test 5 consisted of three samples: two samples of aged GNS frombarrel surrounded by Film No. 22 (0% COC, tight with heat shrink wrap)and one control sample (barrel not wrapped). This test was conducted inclear cups, and the panelists were instructed to evaluate color only.Otherwise, this test was conducted following the protocol and proceduresabove.

Triangle Test 6 consisted of three samples: two samples of GNS from thebarrel wrapped in Film No. 20 (18% COC, tight with heat shrink wrap) andone control sample (barrel not wrapped). This test was conducted inclear cups, and the panelists were instructed to evaluate color only.Otherwise, this test was conducted following the protocol and proceduresabove.

Results of Triangle Test 1 (aged GNS from Control barrel vs. aged GNSfrom barrel surrounded by Film No. 20): The hypothesis can be rejectedbecause less than 10 panelists selected the correct different sample. Inthe black cups, only 6 of the 18 panelists were able to select theControl sample from the sample aged in the barrel surrounded by Film No.20.

Results of Triangle Test 2 (aged GNS from Control barrel vs. aged GNSfrom barrel surrounded by Film No. 22): The hypothesis can be rejectedbecause less than 10 panelists selected the correct different sample. Inthe black cups, only 9 of the 18 panelists were able to select theControl sample from the sample aged in the barrel surrounded by Film No.22.

Results of Triangle Test 3 (aged GNS from Control barrel vs. aged GNSfrom barrel surrounded by Film No. 16): The hypothesis can be acceptedbecause more than 10 panelists selected the correct different sample.Even with the black cups, 12 of the 18 panelists were able to select theControl sample from the sample aged in the barrel surrounded by Film No.16.

Results of Triangle Test 4 (aged GNS from Control barrel vs. aged GNSfrom barrel surrounded by Film No. 20): The hypothesis can be acceptedbecause 17 of the 18 panelists selected the correct different sample. Inthe clear glass cups, only 1 of the 18 panelists was unable, based oncolor alone, to select the Control sample from the sample aged in thebarrel surrounded by Film No. 20.

Results of Triangle Test 5 (aged GNS from Control barrel vs. aged GNSfrom barrel surrounded by Film No. 22): The hypothesis can be acceptedbecause 16 of the 18 panelists selected the correct different sample. Inthe clear glass cups, only 2 of the 18 panelists were unable, based oncolor alone, to select the Control sample from the sample aged in thebarrel surrounded by Film No. 22.

Results of Triangle Test 6 (aged GNS from Control barrel vs. aged GNSfrom barrel surrounded by Film No. 16): The hypothesis can be acceptedbecause 17 of the 18 panelists selected the correct different sample. Inthe clear glass cups, only 1 of the 18 panelists was unable to selectthe Control sample from the sample aged in the barrel surrounded by FilmNo. 16.

Below is a summary of the aroma and taste only Triangle Test Resultsfrom Consumer Panel Test No. 3.

Triangle Test Results for Aroma and Taste Only from Consumer Panel TestNo. 3

Detectable difference of Triangle taste and aroma compared Test No.Treatment to the control — Control Unwrapped N/A 1 Control vs. Film No.20 NO (6/18)* (18% COC) 2 Control vs. Film No. 22 NO (9/18)* (0% COC) 3Control vs. Film No. 16 YES (12/18)* (100% PPS) *The consumer tastepanel had eighteen panelists. For a significant difference of p = 0.05between samples and acceptance of the hypothesis a minimum of 10panelist need to detect a difference by selecting the correct“different” sample (Meilgaard, Civille and Carr, 1991)

Below is a summary of the color only Triangle Test Results from ConsumerPanel Test No. 3.

Triangle Test Results for Color Only from Consumer Panel Test No. 3

Detectable difference of Triangle color compared Test No. Treatment tothe control — Control Unwrapped N/A 4 Control vs. Film No. 20 YES(17/18)* (18% COC) 5 Control vs. Film No. 22 YES (16/18)* (0% COC) 6Control vs. Film No. 16 YES (17/18)* (100% PPS) *The consumer tastepanel had eighteen panelists. For a significant difference of p = 0.05between samples and acceptance of the hypothesis a minimum of 10panelist need to detect a difference by selecting the correct“different” sample (Meilgaard, Civille and Carr, 1991)

The results above from Panel Test No, 3 demonstrated that color was theattribute contributing to the significant difference observed in PanelTest No. 2. The second panel found only the PPS treatment wassignificantly different in taste/smell compared to the control. Allsamples were still significantly different from the control when colorwas evaluated. The data from Panel Test No. 3 demonstrates that bothFilm No. 20 and Film No. 22 exhibited aroma and taste characterindistinguishable from the Control sample.

Sensory Consumer Taste Panel Test No. 4 Barrel Treatment Weights andPercentage “Angel Share” Loss in Barrels Used in Panel Test 5

Average Average Average Average Barrel Initial Final Weight PercentageTreatment weight (g) weight (g) Loss (g) Weight Loss Control 1700.271442.01 258.265 15.19 (unwrapped) Film No. 19 1718.02 1716.16 1.87 0.11Film No. 40 1835.69 1834.92 0.77 0.04 Film No. 39 1801.05 1773.37 27.681.54

Three triangle tests were conducted in order to evaluate if a differencein color, aroma or taste exists between virgin wheat whiskey (VWW)samples aged in control barrels (unwrapped) and VWW aged in barrelswrapped in Film No. 19, Film No. 39 (PVC, as per the prior art) and FilmNo. 40 (Foil, as per the prior art). All of the 1-liter barrels had beenaged about 2 months.

Four one-liter oak barrels were weighed prior to sampling in order tocalculate angel share reduction. The barrels were then agitated forthree minutes. All samples were collected in a commercially sterilemethod and all equipment was cleaned and sanitized prior to use.Separate equipment was used for each sample to preventcross-contamination between samples. Samples were stored in glass jarswith paraffin wrapped around the closure. Jars were then placed in foilbags to prevent both oxygen and light from entering. 800 Milliliters ofaged VWW was collected from each barrel: 100 milliliters for prooftesting, 500 milliliters for sensory testing, and 200 milliliters foranalytical testing. Analytical testing samples were stored in ambervials with paraffin wrapped around the closure.

The GNS samples collected were also submitted to the analytical lab foridentification testing to determine if a difference in compoundsdeveloped during maturation exists between the four samples. Theanalytical lab tested for presences of the following compounds;vanillin, eugenol, syringaldehyde, guaiacol, cresol isomers,coniferaldehyde, syringol, 4-methylguaiacol, s-hydroxymethyl furan,pyrogallol, sinapinaldehyde, methoxy eugenol, acetosyringone, benzoicacid, methyl homovanillate, syringic acid, 4-methyl guaiacol, 4-methylsyringol, 4-vinyl guaiacol, hexadecanoic acid, octadecanoic acid,ellagic acid, o-trimethyl ellagic acid, quercetin, furfural(2-furanaldehyde), whiskey lactone, 5-furancarboxaldehyde, guaiacylacetone, hexose, beta-d-glucopyranose and methyloctalactones. The labalso tested the pH of the samples.

The Standard Guide for Sensory Evaluation of Beverages ContainingAlcohol ASTM E1879-00 was used for the study execution. The panel was aconvenient sample of typical consumers. A brief presentationexplaining/teaching general sensory practices occurred prior to thestudy. Clear cups were used for the sensory testing, so the panelistscould compare sample color differences.

Each triangle test had separate evaluation sheets with different samplecodes. All codes were randomly selected and assigned to treatments. Eachpanelist was also assigned a number, and the serving order of the threetriangles tests was randomized.

The panelists were asked to evaluate the color of the product first,followed by aroma and finally, taste, as in Panel Test No. 1. Panelistswere also asked the same questions as described above in Panel TestNo. 1. However, unlike Panel Test No. 1, the samples were not diluteddown to an ABV of about 30 percent for the sensory studies. The sampleshad an ABV of at least at least 57 percent.

Triangle Test 1 consisted of three samples: two samples from the barrelwrapped in Film No. 19, and one Control sample (barrel not wrapped).This test was conducted following the protocol and procedures above.

Triangle Test 2 consisted of three samples: two samples from the barrelwrapped in Film No. 40 (Foil), and one Control sample (barrel notwrapped). This test was conducted following the protocol and proceduresabove.

Triangle Test 3 consisted of three samples: two samples from the barrelwrapped in Film No. 39 (PVC), and one Control sample (barrel notwrapped). This test was conducted following the protocol and proceduresabove.

The table below, provides a summary of all three triangle tests forConsumer Panel Test No. 4. As can be seen in the table below, the numberof correct responses for the aroma and taste test results was not highenough to show that the panelists could determine differences betweenthe Control sample (unwrapped) and the samples from barrels surroundedby Film Nos. 19, 40, and 39.

Triangle Test Results for Taste and Aroma from Consumer Panel Test No. 4

Detectable difference of Triangle aroma and taste compared Test No.Treatment to the control — Control Unwrapped N/A 1 Control vs. Film No.19 NO (4/8)* 2 Control vs. Film No. 40 NO (3/8)* 3 Control vs. Film No.39 NO (4/8)*

However, it was apparent that the panelists were able to detect thedifference in color of the control sample versus the samples frombarrels surrounded by Film Nos. 19, 40, and 39.

Detectable difference of Triangle color compared Test No. Treatment tothe control — Control Unwrapped N/A 4 Control vs. Film No. 19 YES (7/8)*5 Control vs. Film No. 40 YES (8/8)* 6 Control vs. Film No. 39 YES(7/8)* *Source Meilgaard, Civille and Carr (1991)

The consumer taste panel had eight panelists. For a significantdifference of p=0.05 between samples and acceptance of the hypothesis aminimum of 6 panelist need to detect a difference by selecting thecorrect “different” sample.

Sensory Consumer Taste Panel Test No. 5

It was surmised that in Panel Test No. 4, the alcohol concentration ineach of the samples was so high (ASV of at least 57%) the panelists'senses were overwhelmed by the ABV of the samples, and thereby could notdistinguish one sample from another. Accordingly, another panel wasassembled and the aged VWW samples were tested again. As there wasenough VWW remaining after the completion of Panel Test No. 4, the ageddistillate used in Panel Test No. 5 was taken from the glass containersused to supply and store the aged distillate used in Panel Test No. 4.However, due to the high sample ABV of at least 57% and the concerns ofoverwhelming the panelist's senses as in Panel Test No. 4, the sampleswere diluted 50/50 using demineralized water, in accordance with ASTME1879-00, to achieve an ABV of about 30%.

Also, due to concerns that panelists could utilize color difference toidentify the correct Control sample, black cups were utilized for thearoma and taste test so that color was eliminated as a basis forpanelists' selection of the correct Control sample. Both the aroma andflavor triangle tests of Panel Test No. 5, and color triangle tests thePanel Test No. 5, were conducted in accordance with ASTM E1879-00.

Panel Test No. 5 included a total of six triangle tests. In triangletests 1-3, samples were served in black cups to remove panelist bias forcolor, and the panelists were only allowed to evaluate taste and smell.In triangle tests 4-6, the panelists evaluated color only, and thesamples were served in clear cups.

All samples were stored at room temperature and color coded with tissuepaper to prevent panelist bias during pouring. All samples were servedin 1 oz plastic vials. Panelists were provided with unsalted crackersand water to cleanse their palates, and spit cups were provided.

The table below, summarizes the parameters measured before collectingsamples for analytical testing and sensory testing. Each barrel wasweighed prior to agitation and initial samples were then collected forproof measurements, where the temperature was monitored.

Triangle Test 1 consisted of three samples: two samples from the barrelwrapped in Film No. 19, and one control sample (barrel not wrapped).This test was conducted in black cups with panelists evaluating onlytaste and smell.

Triangle Test 2 consisted of three samples: two samples from the barrelwrapped in Film No. 40 (Foil) and one control sample (barrel notwrapped). This test was conducted in black cups evaluating only tasteand smell.

Triangle Test 3 consisted of three samples: two samples from the barrelwrapped in Film No. 39 (PVC) and one control sample (barrel notwrapped). This test was conducted in black cups evaluating only tasteand smell.

The table below, provides a summary of the results of Aroma and TasteTriangle Tests 1-3 in Panel Test No. 5.

Triangle Test Results for Aroma and Taste from Consumer Panel Test No. 5

Detectable difference of Triangle aroma and taste compared Test No.Treatment to the control — Control Unwrapped N/A 1 Control vs. Film No.19 NO (7/18)* 2 Control vs. Film No. 40 YES (10/18)* 3 Control vs. FilmNo. 39 YES (10/18)*

The consumer test panel had 18 panelists. For a significant differenceof p=0.05 between samples and acceptance of the hypothesis a minimum of10 panelists need to detect a difference by selecting the correctdifferent sample (Miilgaard, Civille and Carr, 1991). In Triangle Test1, the hypothesis can be rejected because less than 10 panelistsselected the correct different sample. In Triangle Test 2, thehypothesis can be accepted because 10 panelists selected the correctdifferent sample. In Triangle Test 3, the hypothesis can be acceptedbecause 10 panelists selected the correct different sample.

Turning next to the Triangle Tests directed to distinguishing samplesbased on color alone, Triangle Test 4 consisted of three samples: twosamples from the barrel wrapped in Film No. 19 and one control sample(barrel not wrapped). This test was conducted in clear cups evaluatingonly color. Triangle Test 5 consisted of three samples: two samples fromthe barrel wrapped in foil and one control sample (barrel not wrapped).This test was conducted in clear cups evaluating only color. TriangleTest 6 consisted of three samples: two samples from the barrel wrappedin PVC and one control sample (barrel not wrapped). This test wasconducted in clear cups evaluating only color.

The table below, provides a summary of the results of Triangle Tests 4-6in Panel Test No. 5.

Triangle Test Results for Color Only from Consumer Panel Test No. 5

Detectable difference of Triangle color compared Test No. Treatment tothe control — Control Unwrapped N/A 4 Control vs. Film No. 19 NO (5/18)*5 Control vs. Film No. 40 YES (18/18)* 6 Control vs. Film No. 39 YES(17/18)*For a significant difference of p=0.05 between samples and acceptance ofthe hypothesis a minimum of 10 panelists need to detect a difference byselecting the correct different sample (Miilgaard, Civille and Carr,1991)

In Triangle Test 4, the hypothesis can be rejected because less than 10panelists selected the correct different sample (Control). In TriangleTest 5, the hypothesis can be accepted because more than 10 panelistsselected the correct different sample. Eighteen panelists were able todetect a difference by identifying the different sample (Control). InTriangle Test 6, the hypothesis can be accepted because more than 10panelists selected the correct different sample. Seventeen panelistswere able to detect a difference by identifying the different sample(Control).

Comparing the results from Panel Tests 4 and 5 demonstrates that thepanelists' senses were overwhelmed by the high ABV of the samples testedin Panel Test 4. The panelists could not distinguish the samples inPanel Test 4 but could distinguish them in Panel Test 5, in which theaged VWW was diluted 50% with water before being consumed by thepanelists.

The results from the Panel Test 5 tests 1-3 established that the Foilbased film of the prior art and the PVC based film of the prior artresult in aroma and taste that is distinguishable from the Control,whereas the working example is not distinguishable from the Control withrespect to aroma and taste. Furthermore, the results from Panel Tests4-6 established that the barrel surrounded by the Foil based film of theprior art and the barrel surrounded by the PVC film of the prior artresult in color differences distinguishable from the Control, whereasthe working example produces color which is not distinguishable from thecontrol. Moreover, with respect to the barrel surrounded by Film No. 19,panelists were unable to detect a significant difference between theworking example and the Control with respect to color, aroma, and taste.

The table below is a compilation of the results angel share weight losstests and the sensory panel tests set forth above. Also provided arephysical properties for the films used in the tests, including varioustransmission rates, impact strength, and elongation to break.

The sensory panel tests results show that the alcoholic beverages agedin barrels surrounded by Film Nos. 19, 20, and 22 resulted in an agedproduct having an aroma and flavor indistinguishable from the control.The alcoholic beverage aged in Film No. 19 was the only aged alcoholicbeverage indistinguishable from the control with respect to aroma,flavor, and color.

Various comparative films included Film No. 16, Film No. 37, Film No.39, and Film No. 40, each of which was used to produce an aged alcoholicbeverage that the sensory panel was able to distinguish from thecontrol.

Although Film Nos. 18, 24, 25, 34, and 38 were not subjected to thesensory panel test, the permeabilities and presence ofethylene/norbornene were in common with Film No's 19 and 20, and wouldmake Film Nos. 18, 24, 25, 34, and 38 likely to produce sensory panelresult similar to the sensory panel results for Film Nos. 19 and 20.

Film No. 16, although having the requisite permeability combination,produced an off flavor component DEHP as shown in the pyrolysis-GCMStesting reported below.

Permeabilities, Peak Load, Elongation to Break, Angels' Share, andSensory Data for Various Films

Permeabilities Angel Share Loss Film No. Ethanol Moisture (wt %) SensoryTest & Transmission Vapor Peak 5 Gallon Aroma and Film Rate OxygenTransmission Load Elongation Barrel* 1 Liter Taste Color Thickness wt %(ETR) Transmission Rate (New- to Break (gns aged Barrel DifferenceDifference (mils) COC (Mocon) Rate (OTR) (MVTR) tons) (Joules) 398 days)Test 1 to Control to Control Control — — — — — — 6.6 10.0  — —(Unwrapped Barrel) #16 6 mils 0 0.032 21.2 0.91 — — 2.8 — Yes Yesg/m²/day cc/m²/day g/m²/day #18: 3 mils 35 — 264 0.663 177 2.15 1.7 — —— cc/m² /day g/m²/day #19: 3 mils 49 0.217 209 0.54 180 2.07 0.3 0.22 NoNo (working) g/m²/day cc/m²/day g/m²/day @ 49 days aging #20: 2.01 mils18 — — — — — 0.7 — No Yes (working) (lighter) #22: 2.01 mils 0 18.3 2650.5 286 4.02 1.2 0.53 No Yes (working) g/m²/day cc/m²/day g/m²/day(lighter) #24: 2.5 mils 20 0.41 250 0.66 175 2.18 — — — — (Working)g/m²/day cc/m²/day g/m²/day #25: 2.5 mils 28 0.32 262 0.71 167 1.77 —0.13 — — (working) g/m²/day cc/m²/day g/m²/day #34: 6 mils 21.7 0.25 2920.19 — — — — — — g/m²/day cc/m²/day g/m²/day #36: 1.56 mils 0 0.22 32.110.6 158 0.69 — 0.88 — — (comparative) g/m²/day cc/m²/day g/m²/day #37:1.2 mil 0 8.3 33 24.7  75 0.55 2.3 — Yes — (comparative) g/m²/daycc/m²/day g/m²/day #38: 4.5 mils 18 0.84 283 0.62 — — — — — — g/m²/daycc/m²/day g/m²/day #39: 2.5 mil 0 8.41 230 1.36 — — — 1.54 Yes Yes(comparative) g/m²/day cc/m²/day g/m²/day @ 49 days Aging #40: 4.5 mils0 <0.1 <0.1 0.1 — — — 0.04 Yes Yes Coated @ 49 days Metal Foil aging(comparative)

TDU-Pyrolysis GCMS Testing to Identify Volatiles and Semi-VolatilesGenerated During Whisky Maturation

Four 1-liter wooden oak barrels were filled with a virgin wheat whiskey(VWW) distillation product, and aged for two months at ambientconditions. The first barrel was not wrapped with film and was theControl barrel. The second barrel was surrounded by Film No. 19. Thethird barrel was surrounded by Film No. 40. The fourth barrel wassurrounded by Film No. 39.

After the two-month aging period, samples were taken from each of thefour barrels and placed in 4 ounce amber bottles. Analysis of thesamples in the bottles was carried out using an Agilent 6890N GasChromatograph (GC) equipped with a 5975C Mass Selective Detector (MSD)and a GERSTEL Cooled Injection System (CIS 4) which was a programmedtemperature vaporization (PTV) type inlet with liquid nitrogen cooling(LN₂). Sample introduction was automated using a GERSTEL MultiPurposeSampler (MPS) equipped with a GERSTEL Thermal Desorption Unit (TDU)containing the pyrolysis insert, GERSTEL PYRO. The TDU-PYRO was coupleddirectly to the CIS 4 inlet.

The objective was to carry out analytical testing for the purpose ofdetermining how different films surrounding the barrel during agingaffected the composition of the aged distillate product inside thebarrels surrounded by Film No. 19 (working example), Film No. 39(comparative example in accordance with prior art), and Film No. 40(comparative example in accordance with prior art) versus the ageddistillate from a Control barrel having no film around it.

More particularly, the aged distillate in each barrel was tested for theamount of specific compounds, including vanillin, guaiacol,syringaldehyde, syringol, eugenol, isoeugenol,cis-β-methyl-γ-octalactone, o-cresol, 2-methoxy-4-methylphenol,4-methylsyringol, 4-ethylguaiacol, 4-vinylguaiacol, vanillyl methylketone, methoxyeugenol, sinapaldehyde, and furfural. These compounds areknown to impart desirable aroma, flavor, and color characteristics tothe distillate as it ages. These compounds are either extracted from thewooden of the barrel or are reaction products of extracts from thewooden making up the barrel. In addition, the third objective wascarried out for di(2-ethylhexyl)phthalate (“DEHP”), which is anunfavorable aroma.

Twenty microliters of each of the aged whiskey samples were pipettedseparately into short, quartz test-tube shaped pyrolysis vials withslits using a manual microliter syringe. The tubes were secured withglass wool, connected to pyrolysis adapters and placed into a 98position pyrolysis tray in the MPS. The whiskey samples were thermallydesorbed at 300° C. to remove the volatile and semi-volatile compounds.Following thermal desorption, the samples were pyrolyzed at 450° C. toget the maximum amount of information from each sample.

-   -   The analytical conditions were as follows:

Pyrolysis: 450° C.; Lead Time: 0.10 min; Follow up Time: 1.0 min;Initial Time: 0.5 min TDU: Splitless; 40° C. (0.2 min.); 720° C./min to300° C. (3 min) PTV: Quartz liner; Solvent vent (100 mL/min); 40° C.(0.05 min.); 10° C./s to 300° C. (10 min) Column: 30 m HP-5MS (Agilent);d_(i) = 0.25 mm; d_(f) = 0.25 μm Pneumatics: He, constant flow @ 1.5milliliters/min Oven: 35° C. (3 min); 10° C./min to 315° C. (10 min)MSD: EI mode; full scan; 35-650 amu

FIGS. 29-45 provide the results of the above GC/MS analytical testingfor, respectively: vanillin, guaiacol, syringaldehyde, syringol,eugenol, isoeugenol, cis-β-methyl-γ-octalactone, o-cresol,2-methoxy-4-methylphenol, 4-methylsyringol, 4-ethylguaiacol,4-vinylguaiacol, vanillyl methyl ketone, methoxyeugenol, sinapaldehyde,furfural, and di(2-ethylhexyl)phthalate (“DEHP”) in the barrelssurrounded by Film Nos. 19, 39, and 40, as well as for the controlbarrel. Film No. 19 was a preferred film having three layers, with thecore layer made from a blend containing 70 wt % ethylene norbornenecopolymer, which is a cyclic olefin copolymer. Film No. 19 contained thecyclic olefin copolymer in an amount of 49 wt %, based on total filmweight.

In FIGS. 29-44, a comparison of the amount of various desirable aromaand flavor components in the aged distillate in the barrel surrounded byFilm No. 19 was more than 50 percent of the amount of the same aroma andflavor components in the aged distillate in the control barrel. In viewof the much lower levels of the same flavor components produced by PVC(Film No. 39) and the foil-based film (Film No. 40), these results wereunexpected. Moreover, FIGS. 29-44 show that the amount of the variousdesirable aroma and flavor components in the aged distillate from thebarrel surrounded by Film No. 19 were present at a level of more than 75percent of the amount of the same aroma and flavor components in theaged distillate in the control barrel, which was yet a further level ofunexpectedness.

In FIGS. 32 (syringol), 33 (eugenol), 35 (cis-β-methyl-γ-octalactone),36 (o-cresol), 37 (2-methoxy-4-methylphenol), 38 (4-methylsyringol), 39(4-ethylguaiacol), 41 (vanillyl methyl ketone), 42 (methoxyeugenol), and44 (furfural), the amount of the aroma and flavor component in the ageddistillate from the barrel surrounded by Film No. 19 exceeded the amount(i.e., was unexpectedly more than 100% of the amount) of thecorresponding aroma and flavor component in the control distillate agedwithout a film around the barrel. This result is of further significancebecause it suggests that the presence of the film produced acceleratedaging of these specific aroma and flavor components by producing thesearoma and flavor components at a faster rate. This has the potential toproduce aged distillates of enhanced quality and/or accelerated agingrate.

In contrast to the aged distillate from the barrel surrounded by FilmNo. 19 and the control distillate aged without a film around the barrel,FIGS. 29-44 show that the aged distillates from the barrels surroundedby Film No. 39 (PVC-in accordance with the prior art) and Film No. 40(coated metal foil in accordance with prior art) produced less than halfof the flavor components of the control distillate. In most cases, FilmNos. 39 and 40 produced less than 25 percent of the flavor components ofthe control distillate. In two cases (FIG. 33: eugenol; FIG. 34:isoeugenol), the flavor component in the aged distillates from thebarrels surrounded by Film No. 39 (PVC) and Film No. 40 (Foil) was lessthan 10 percent of the same flavor component in the working exampleutilizing Film No. 19.

Finally, FIG. 45 shows that the aged distillate from the barrelsurrounded by Film No. 39 (100% polyvinylchloride (PVC)), contained arelatively high amount of di(2-ethylhexyl)phthalate (DEHP), a compoundproviding an unfavorable aroma. This is believed to be at least part ofthe reason that panelists were able to detect a difference between thealcoholic beverage aged in Film No. 39 versus the alcoholic beveragesaged in Film Nos. 19, 20, and 22.

Although the present invention has been described with reference to thepreferred embodiments, it is to be understood that modifications andvariations of the invention exist without departing from the principlesand scope of the invention, as those skilled in the art will readilyunderstand. Accordingly, such modifications are in accordance with theclaims set forth below.

What is claimed is:
 1. A process for aging an alcoholic beverage,comprising: (A) filling a first wooden barrel with an unaged alcoholicbeverage, the barrel having an outer surface; (B) covering at least 60percent of the outer surface of the first wooden barrel with a filmhaving an oxygen transmission rate of at least 50 cc/m²/day and anethanol transmission rate of less than 30 g/m²/day; (C) aging the unagedalcoholic beverage under ambient conditions while the alcoholic beverageremains in the first wooden barrel surrounded by the film for a timeperiod of at least 1 month, to produce an aged alcoholic beverage, andwherein during aging, the alcoholic beverage acquires or produces atleast one flavor component selected from the group consisting ofvanillin, guaiacol, syringaldehyde, syringol, eugenol, isoeugenol,cis-β-methyl-γ-octalactone, o-cresol, 2-methoxy-4-methylphenol,4-methylsyringol, 4-ethylguaiacol, 4-vinylguaiacol, vanillyl methylketone, methoxyeugenol, sinapaldehyde, and furfural, so that the agedalcoholic beverage contains the at least one flavor component in anamount of at least 50% relative to an amount of the same flavorcomponent in a control alcoholic beverage aged in a control woodenbarrel without any film covering the control barrel during aging.
 2. Theprocess according to claim 1, wherein at least 75% of the outer surfaceof the first wooden barrel is covered with the film, and the agedalcoholic beverage contains the at least one flavor component in anamount of at least 75% relative to the amount of the same flavorcomponent in the control alcoholic beverage.
 3. The process according toclaim 2, wherein the aged alcoholic beverage contains each flavorcomponent in the group consisting of vanillin, guaiacol, syringaldehyde,syringol, eugenol, isoeugenol, cis-β-methyl-γ-octalactone, o-cresol,2-methoxy-4-methylphenol, 4-methylsyringol, 4-ethylguaiacol,4-vinylguaiacol, vanillyl methyl ketone, methoxyeugenol, sinapaldehyde,and furfural in an amount of at least 75% relative to the amount of eachcorresponding flavor component in the control alcoholic beverage.
 4. Theprocess according to claim 1, wherein the film surrounds the outersurface of the first wooden barrel, and the aged alcoholic beveragecontains each flavor component in the group consisting of each ofsyringol, eugenol, cis-β-methyl-γ-octalactone, o-cresol,2-methoxy-4-methylphenol, 4-methylsyringol, 4-ethylguaiacol, vanillylmethyl ketone, and furfural in an amount of more than 100% relative tothe amount of each corresponding flavor component in the controlalcoholic beverage.
 5. The process according to claim 1, wherein thefilm surrounds the outer surface of the first wooden barrel, and thefilm comprises cyclic olefin copolymer in an amount of from 15 to 80weight percent, based on total film weight, and wherein the film has athickness of from 1.5 to 6 mils, and wherein the aged alcoholic beveragecontains eugenol in an amount of at least 110% relative to the amount ofeugenol in the control alcoholic beverage.
 6. The process according toclaim 1, wherein the film comprises cyclic olefin copolymer in an amountof from 15 to 80 weight percent, based on total film weight, and thefilm has a thickness of from 1.5 to 6 mils and an ethanol transmissionrate of less than 1 g/m²/day and an oxygen transmission rate of at least170 cc/m²/day.
 7. The process according to claim 1, wherein the film isa multilayer film comprising polyolefin in an amount of from 50 to 82percent, based on total film weight, and cyclic olefin copolymer in anamount of from 18 to 50 weight percent based on total film weight, withthe cyclic olefin copolymer being present in a blend with polyolefin,the film having a thickness of from 1.5 to 4 mils.
 8. The processaccording to claim 7, wherein the multilayer film comprises three layersincluding two outer layers and one inner layer, the inner layercomprising a blend of from 20 to 80 wt % ethylene norbornene copolymerand from 80 to 20 wt % ethylene/alpha-olefin copolymer, and thealcoholic beverage product is selected from distillate and wine.
 9. Theprocess according to claim 8, wherein the barrel is surrounded by thefilm and the film has an ethanol transmission rate of less than 1g/m²/day and an oxygen transmission rate of at least 170 cc/m²/day and amoisture vapor transmission rate less than 1 g/m²/day, and the agedalcoholic beverage, either having an alcohol by volume of less than 30%or being diluted with water to have an alcohol by volume of 30%,exhibits an aroma and flavor, evaluated in accordance with ASTM E1879-00Sensory Evaluation of Beverages Containing Alcohol, and ASTM E1885-04Standard Method for Sensory Analysis—Triangle Test, indistinguishablerelative to the control barrel containing the control alcoholicbeverage.
 10. The process according to claim 9, wherein the inner layercomprises a blend of from 40 to 60 wt % ethylene norbornene copolymerand from 60 to 40 wt % polyolefin, and the film has a thickness of from2 to 3.5 mils and an ethanol transmission rate of less than 0.5 g/m²/dayand an oxygen transmission rate of at least 170 to 250 cc/m²/day, andthe first aged alcoholic beverage, either having an alcohol by volume ofless than 30% or being diluted with water to have an alcohol by volumeof 30%, further exhibits a color, evaluated in accordance with ASTME1879-00 Sensory Evaluation of Beverages Containing Alcohol, and ASTME1885-04 Standard Method for Sensory Analysis—Triangle Test,indistinguishable relative to the control barrel containing the controlalcoholic beverage.
 11. A process for aging an alcoholic beverage,comprising: (A) filling a first wooden barrel with the unaged alcoholicbeverage, the barrel having an outer surface; (B) covering at least 60percent of the outer surface of the first wooden barrel with a filmhaving an oxygen transmission rate of at least 50 cc/m²/day and anethanol transmission rate of less than 30 g/m²/day; and (C) aging theunaged alcoholic beverage in the first wooden barrel covered with thefilm, the aging being carried out under ambient conditions for a timeperiod of at least 1 month while the alcoholic beverage remains in thefirst wooden barrel covered by the film, to produce an aged alcoholicbeverage, wherein during aging an angel share fraction of the alcoholicbeverage escapes through the wooden barrel and through the film coveringthe outer surface of the wooden barrel, with the angel share fractionbeing at least 30% less relative to a corresponding angel share fractionescaping through a wooden control barrel containing a control alcoholicbeverage aged in the control barrel, the control barrel having an outersurface in direct contact with an ambient atmosphere without any filmcovering any portion of the control barrel; and wherein the agedalcoholic beverage, either having an alcohol by volume of less than 30%or upon being diluted with water to have an alcohol by volume of 30%,exhibits an aroma and flavor, upon evaluation in accordance with ASTME1879-00 Sensory Evaluation of Beverages Containing Alcohol togetherwith ASTM E1885-04 Standard Method for Sensory Analysis—Triangle Test,indistinguishable relative to the control barrel containing the controlalcoholic beverage aged therein, the aged control alcoholic beveragealso having an alcohol by volume of less than 30% or being diluted withwater to have an alcohol by volume of 30%.
 12. The process according toclaim 11, wherein the first barrel is surrounded by the film and whereinthe angels' share fraction escaping through the first wooden barrel andthrough the film is at least 70% less than the angel share fractionescaping through the wooden control barrel containing the controlalcoholic beverage, and wherein the film comprises polyolefin.
 13. Theprocess according to claim 11, wherein the first barrel is surrounded bythe film and wherein the angels' share fraction escaping through thefirst wooden barrel and through the film is at least 85% less than theangel share fraction escaping through the wooden control barrelcontaining the control alcoholic beverage, and wherein the filmcomprises from 30 to 85 wt % polyolefin and from 70 to 15 wt %ethylene/norbornene copolymer based on total film weight, and whereinthe film has an oxygen transmission rate of from 170 to 350 cc/m²/dayand an ethanol transmission rate of from 0.10 to 1.0 g/m²/day, and amoisture vapor transmission rate of 0.1 to 0.8 g/m²/day.
 14. The processaccording to claim 13, wherein during aging the angels' share fractionescaping through the first wooden barrel and through the film is atleast 90% less than the angel share fraction escaping through the woodencontrol barrel containing the control alcoholic beverage, and whereinthe film comprises from 40 to 60 wt % polyolefin and from 60 to 40 wt %ethylene/norbornene copolymer based on total film weight, and whereinthe film has an oxygen transmission rate of from 170 to 250 cc/m²/dayand an ethanol transmission rate of from 0.17 to 0.27 g/m²/day, andwherein the aged alcoholic beverage, either having an alcohol by volumeof less than 30% or being diluted with water to have an alcohol byvolume of 30%, further exhibits a color, evaluated in accordance withASTM E1879-00 Sensory Evaluation of Beverages Containing Alcohol, andASTM E1885-04 Standard Method for Sensory Analysis—Triangle Test,indistinguishable relative to the control barrel containing the controlalcoholic beverage.
 15. A process for aging an alcoholic beverage,comprising: (A) filling a wooden barrel with an unaged alcoholicbeverage, the wooden barrel having an oxygen transmission rate of from 1to 10 cc/m²/day; (B) covering an outer surface of the barrel with a filmhaving an oxygen transmission rate of at least 50 cc/m²/day and anethanol transmission rate of less than 30 g/m²/day, the film having athickness of from 1 to 10 mils; and (C) aging the unaged alcoholicbeverage while it remains in the wooden barrel, covered by the film, forat least 1 month, to produce an aged alcoholic beverage.
 16. The processaccording to claim 15, wherein the film has an oxygen transmission rateof at least 100 cc/m²/day and an ethanol transmission rate of from 0.1to 20 g/m²/day, and the film comprises polyolefin.
 17. The processaccording to claim 11, wherein the film has a thickness of from 1.5 to 5mils.
 18. The process according to claim 16, wherein the film has anoxygen transmission rate of at least 120 cc/m²/day and an ethanoltransmission rate of 0.1 to 1 g/m²/day, and the film further comprises acyclic olefin copolymer, and the aging of the alcoholic beverage iscarried out for at least 2 months.
 19. The process according to claim18, wherein the film further comprises a blend of the polyolefin and thecyclic olefin copolymer, and the cyclic olefin copolymer comprisesethylene/norbornene copolymer, and the ethylene norbornene copolymer ispresent in the film in an amount of from 15 to 70 weight percent basedon total film weight and the polyolefin is present in the film in anamount of from 30 to 85 wt % based on total film weight, and the agingof the alcoholic beverage is carried out for at least 3 months, and thefilm has a thickness of from 2 to 4 mils, an oxygen transmission rate offrom 150 to 500 cc/m²/day, an ethanol transmission rate of less than 1g/m²/day, and a moisture vapor transmission rate less than 1 g/m²/day.